<a href="https://www.the-hive.ws/forum/showflat.pl?Number=68385&page=21&view=&sb=&Search=&vc=&new=&start=0&xrated=y&&URLForums=" title="Click here to show this downrated post">Catalytic Hydrogenation of Ephedrine</a> (Rated as: misinforming) </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post68432"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> C10H15N (Stranger) 11-10-00 08:43 No 68432 </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> Re: Catalytic Hydrogenation...... </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> -ok 3%,5% or 10% is fine. Pd/C is a catalyst, witch means that your 5% will only make things go quicker. <hr>its only a matter of time.<img src="../forum/images/icons_lightgrey/cool.gif" alt="cool" title="Cool" heigth="15" width="15"> </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post68443"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> bumblebeetuna (Stranger) 11-10-00 09:46 No 68443 </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> Re: Catalytic Hydrogenation...... </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> ok, any ideas on making pressurised h2? I was thinking conc H2SO4 + Mg inside on old oxygen tank with a pressure gauge....I gues i would have to know the exact cap of the tank, ... even then is that really safe???? </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post68504"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> terbium (Hive Bee) 11-10-00 13:39 No 68504 </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> Re: Catalytic Hydrogenation...... </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> It is stainless steel not steal. It is hydrogenate not hydrate There are several procedures on Rhodium's site that have serious errors or, IMHO, just plain won't work. This procedure for hydrogenating ephedrine is one of them. I like the part about sucking the air out of the vessel by "mouth suction" - ROTFLOL! Most people wouldn't even use vacuum to rid the reactor of air - even if they had something better than mouth suction. Instead purge with nitrogen to remove the oxygen then purge with hydrogen to remove the nitrogen. </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post68508"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> Ballistic (Stranger) 11-10-00 13:47 No 68508 </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> Re: Catalytic Hydrogenation...... </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> What is the error in this rxn? And how could it be fixed? I was going to try it because it used easy to obtain reagents. <hr> The rain in Maine falls mainly down the drain. </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post68511"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> serodronin (Stranger) 11-10-00 13:54 No 68511 </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> Re: Catalytic Hydrogenation...... </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> this synthesis is a little sketchy, but the concept of it could be modified to make it work. you would have to use chloroephedrine for it to work. there are plenty of better synthesis out there for hydrogenation using palladium catalysts. I personally don't trust any synthesis that I can't find in a patent. You will need more than 30 psi to pull off a reaction like this. I usually shoot for about 60psi(5atm). also, every reaction of this nature I've seen used glacial acetic combined with another strong acid(H2SO4,HClO4, etc.) no everclear mentioned. </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post68514"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> terbium (Hive Bee) 11-10-00 14:01 No 68514 </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> Re: Catalytic Hydrogenation...... </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> There is an old journal article that claims hydrogenation of ephedrine to methamphetamine but they used concentrated HCL, Raney Nickle and high temperature and pressure. I am very suspicious of these claims of doing it in dilute or weak acids and at low temperatures and pressures. </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post68517"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> serodronin (Stranger) 11-10-00 14:06 No 68517 </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> Re: Catalytic Hydrogenation...... </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> I read that article, and I think it was wrong also. they claimed that reducing ephedrine resulted in amphetamine, and reducing norepinephrine produced methamphetamine. this is backwards. here is one I dug up: Kindler et al., The Mechanisms of Chemical Reactions. X. Preparation of Phenyl- and Cyclohexylalkylamines by Hydrogenation. Justus Liebigs Ann. Chem., 560, 215-21 (1948); C.A. 43: 1025g (1949). It was found the hydrogenation of ephedrine to the corresponding amine is faster with strong acids, such as H2SO4 and HClO4. Amino alcohols (such as ephedrine and phenylpropanolamine) were hydrogenated only slowly in the absence of acid. The use of H2SO4-H2O was better than that of H2SO4, avoiding reduction to H2S and catalyst poisoning. The use of HClO4 in large amounts caused reduction of C6H5 to C6H11 (the benzene ring was reduced to a cyclohexane ring). (+)-Phenylisopropylmethylamine (PhCH2CHMeNHMe) was prepared in 95% yield as the crude hydrochloride salt from 4 g. ephedrine hydrochloride, 90 cc. acetic acid, 4.7 g. 84% H2SO4, and 1 g. palladium wool. M.p. 166-8�, m.p. 182� (from chloroform and ethyl acetate). I don't notice any obvious errors in this logic. also, I believe that Pd/C or Pd/BaSO4 would work fine as catalysts. I am assuming that this reaction needs to occur under pressure and with somewhere between 60-90C temperature. </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post68530"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> Ballistic (Stranger) 11-10-00 14:40 No 68530 </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> Re: Catalytic Hydrogenation...... </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> So what you guys are saying is that this rxn produced something but it wasn't meth. All the other rxn of this type did include acetic acid. Would there be something you could substitute for acetic acid that one could produce or acuire without going to a chem store? <hr> The rain in Maine falls mainly down the drain. </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post68534"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> serodronin (Stranger) 11-10-00 14:55 No 68534 </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> Re: Catalytic Hydrogenation...... </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> they make something, but it ain't meth. just gives you a buzzy headache you wish would go away. glacial acetic acid is kept in quantity at photo supply stores. really simple to get, just go in and pay cash. no questions asked. if you're really paranoid or can't find a photo supply store, go to the grocery store and get white vinegar. you can distill it out from there. </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post68550"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> WizardX (Wizard Master) 11-10-00 15:39 No 68550 </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> Re: Catalytic Hydrogenation...... </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> The easiest way to make H2 gas is Aluminium and Sodium hydroxide solution (1M). The H2 gas can then be compressed into a gas cylinder while cooled in ice. </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post68558"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> placebo (irritable and cranky) 11-10-00 17:08 No 68558 </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> Re: Catalytic Hydrogenation...... </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> This is KrZ's write-up called "Mastermind" I believe. I am not sure, but I thought it had been tried and was succeful by others, but I may just have an over-active imagination and a un-natural need to stroke KrZ's ego. I am sure Rhodium would not have put it up on his site if it had no merit and obvious errors. But stranger things have happened! Look at the mole on Stonium's bum. <hr> Wanna do the rumpy pump? </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post68568"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> terbium (Hive Bee) 11-10-00 18:18 No 68568 </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> Re: Catalytic Hydrogenation...... </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <blockquote title="Quoted text"><hr>I am sure Rhodium would not have put it up on his site if it had no merit and obvious errors.<hr></blockquote>How about the catalytic hydrogenation of phenylalanine to amphetamine that is on Rhodium's site. Does anybody really think that that works? <a href="http://rhodium.lycaeum.org/chemistry/phenylalanine.txt" target="_blank" title="Jump to this external site">http://rhodium.lycaeum.org/chemistry/phenylalanine.txt</a> Another one I like is the rP/I reduction procedure that calls for placing the iodine and rP together in a ball mill so that they will be "thoroughly mixed". And then there is the procedure we are discussing here that calls for removing the air from the hydrogenation reactor by "mouth suction". This would be funny if it weren't that some people will actually believe it. </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post68938"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> KrZ (Hallucinogenius) 11-12-00 17:23 No 68938 </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> Re: Catalytic Hydrogenation...... </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> That reaction is an exact duplicate of the reference which someone posted only days before, I will see if I can find it. Mouth suction is a joke for idiot meth cooks, like all those warnings you see about mouth pipetting that are still around today even though it hasn't been done in decades. </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post392325"></a><a name="last"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> Organikum (Hive Addict) 12-23-02 22:40 No 392325 </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> for completeness </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> ok, this is a quite old thread but I want to add something for not misleading bees on search. The german <a href="http://l2.espacenet.com/dips/viewer?PN=DE968545&CY=gb&LG=en&DB=EPD" target="_blank" title="Jump to this patent">Patent DE968545</a> by Knoll AG from 1958 states that the by in post <a href="../crystal/000068385.html#Post68517">Post 68517</a> (serodronin: "Re: Catalytic Hydrogenation......", Stimulants) cited reference <blockquote title="Quoted text"><hr>Kindler et al., The Mechanisms of Chemical Reactions. X. Preparation of Phenyl-and Cyclohexylalkylamines by Hydrogenation. Justus Liebigs Ann. Chem., 560, 215-21 (1948); C.A. 43: 1025g (1949).<hr></blockquote>is wrong as this will not work as described with H2SO4. The patent further describes a ephedrine.HCl reduction with in GAA solved HCl and Pd sponge as catalyst. The catalyst/substrate ratio is insane. The procedure can be modified by using 10%Pd/BaSO4 or 10%Pd/C as catalyst in a much lower ratio and adding small amounts of 70% HClO4 (which has to be diluted in GAA before addition). With this modifications it is a very good yielding synth for clean substrates. ORG <hr><center>now or never</center> </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post507994"></a><a name="last"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> Rhodium (Chief Bee) 05-18-04 13:05 No 507994 </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> Catalytic Hydrogenation of Ephedrine to Meth (Rated as: excellent) </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> �ber die Darstellung von β-Aryl-alkylaminen Karl Wilhelm Rosenmund & Erwin Karg <a href="../rhodium/pdf /ephedrine.hydrogenation.rosenmund.pdf" target="_blank" title="Jump to this external site">Chem. Ber. 75, 1850-1859 (1942)</a> (../rhodium/pdf /ephedrine.hydrogenation.rosenmund.pdf) Mentioned before in: <a href="../DUMMY">Post 71342</a> (serodronin: "Preparation of B-arylalkylamines", Methods Discourse) (Contains english abstract of this article) <a href="../DUMMY">Post 269642</a> (MethKat: "paladium ingot", Stimulants) ____ ___ __ _ Studien �ber den Mechanismus chemischer Reaktionen. X. Phenyl- und Cyclohexyl-alkylamine durch Hydrierung Karl Kindler, Bruno Hedemann, Ernst Sch�rfe <a href="../rhodium/pdf /ephedrine.hydrogenation.kindler.pdf" target="_blank" title="Jump to this external site">Ann. Chem. 560, 215-221 (1948)</a> (../rhodium/pdf /ephedrine.hydrogenation.kindler.pdf) Mentioned before in: <a href="../crystal/000068385.html#Post68517">Post 68517</a> (serodronin: "Re: Catalytic Hydrogenation......", Stimulants) (Contains english abstract of this article) <a href="../DUMMY">Post 359515</a> (Chicken: "This refernce", Stimulants) <a href="../crystal/000068385.html#Post392325">Post 392325</a> (Organikum: "for completeness", Stimulants) <hr>The Hive - Clandestine Chemists Without Borders </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> </body> </html>

Catalytic Hydrogenation of Ephedrine , Hive Stimulants


		bumblebeetuna 11-10-00 04:42				<a href="https://www.the-hive.ws/forum/showflat.pl?Number=68385&page=21&view=&sb=&Search=&vc=&new=&start=0&xrated=y&&URLForums=" title="Click here to show this downrated post">Catalytic Hydrogenation of Ephedrine</a> <br> <i title="This post has been downrated by the moderators">(Rated as: misinforming)</i> </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post68432"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> C10H15N<br> <i>(<span title="The user's title at the time of posting">Stranger</span>)</i><br> <span title="Posting date">11-10-00 08:43</span><br> <span title="Link to this post by using the markup [68432]">No 68432</span><br> </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">Re: Catalytic Hydrogenation......</b> </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> -ok 3%,5% or 10% is fine. Pd/C is a catalyst, witch means<br> that your 5% will only make things go quicker.<br><hr><font color="blue">its only a matter of time.</font color="blue"><img src="../forum/images/icons_lightgrey/cool.gif" alt="cool" title="Cool" heigth="15" width="15"> </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post68443"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> bumblebeetuna<br> <i>(<span title="The user's title at the time of posting">Stranger</span>)</i><br> <span title="Posting date">11-10-00 09:46</span><br> <span title="Link to this post by using the markup [68443]">No 68443</span><br> </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">Re: Catalytic Hydrogenation......</b> </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> ok, any ideas on making pressurised h2? I was thinking conc H2SO4 + Mg inside on old oxygen tank with a pressure gauge....I gues i would have to know the exact cap of the tank, ... even then is that really safe???? </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post68504"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> terbium<br> <i>(<span title="The user's title at the time of posting">Hive Bee</span>)</i><br> <span title="Posting date">11-10-00 13:39</span><br> <span title="Link to this post by using the markup [68504]">No 68504</span><br> </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">Re: Catalytic Hydrogenation......</b> </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> It is stainless <b>steel</b> not <b>steal</b>.<br><br>It is <b>hydrogenate</b> not <b>hydrate</b><br><br>There are several procedures on Rhodium's site that have serious errors or, IMHO, just plain won't work. This procedure for hydrogenating ephedrine is one of them.<br><br>I like the part about sucking the air out of the vessel by "mouth suction" - ROTFLOL!<br><br>Most people wouldn't even use vacuum to rid the reactor of air - even if they had something better than mouth suction. Instead purge with nitrogen to remove the oxygen then purge with hydrogen to remove the nitrogen. </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post68508"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> Ballistic<br> <i>(<span title="The user's title at the time of posting">Stranger</span>)</i><br> <span title="Posting date">11-10-00 13:47</span><br> <span title="Link to this post by using the markup [68508]">No 68508</span><br> </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">Re: Catalytic Hydrogenation......</b> </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> What is the error in this rxn? And how could it be fixed?<br>I was going to try it because it used easy to obtain reagents. <br><hr><br>The rain in Maine falls mainly down the drain. </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post68511"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> serodronin<br> <i>(<span title="The user's title at the time of posting">Stranger</span>)</i><br> <span title="Posting date">11-10-00 13:54</span><br> <span title="Link to this post by using the markup [68511]">No 68511</span><br> </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">Re: Catalytic Hydrogenation......</b> </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> this synthesis is a little sketchy, but the concept of it could be modified to make it work. you would have to use chloroephedrine for it to work. there are plenty of better synthesis out there for hydrogenation using palladium catalysts. I personally don't trust any synthesis that I can't find in a patent. You will need more than 30 psi to pull off a reaction like this. I usually shoot for about 60psi(5atm). also, every reaction of this nature I've seen used glacial acetic combined with another strong acid(H2SO4,HClO4, etc.) no everclear mentioned. </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post68514"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> terbium<br> <i>(<span title="The user's title at the time of posting">Hive Bee</span>)</i><br> <span title="Posting date">11-10-00 14:01</span><br> <span title="Link to this post by using the markup [68514]">No 68514</span><br> </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">Re: Catalytic Hydrogenation......</b> </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> There is an old journal article that claims hydrogenation of ephedrine to methamphetamine but they used concentrated HCL, Raney Nickle and high temperature and pressure. I am very suspicious of these claims of doing it in dilute or weak acids and at low temperatures and pressures. </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post68517"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> serodronin<br> <i>(<span title="The user's title at the time of posting">Stranger</span>)</i><br> <span title="Posting date">11-10-00 14:06</span><br> <span title="Link to this post by using the markup [68517]">No 68517</span><br> </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">Re: Catalytic Hydrogenation......</b> </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> I read that article, and I think it was wrong also. they claimed that reducing ephedrine resulted in amphetamine, and reducing norepinephrine produced methamphetamine. this is backwards. here is one I dug up:<br><br>Kindler et al., The Mechanisms of Chemical Reactions. X. Preparation of Phenyl-<br>and Cyclohexylalkylamines by Hydrogenation. Justus Liebigs Ann. Chem., 560,<br>215-21 (1948); C.A. 43: 1025g (1949).<br><br>It was found the hydrogenation of ephedrine to the corresponding amine is faster<br>with strong acids, such as H2SO4 and HClO4. Amino alcohols (such as ephedrine<br>and phenylpropanolamine) were hydrogenated only slowly in the absence of acid.<br>The use of H2SO4-H2O was better than that of H2SO4, avoiding reduction to H2S<br>and catalyst poisoning. The use of HClO4 in large amounts caused reduction of<br>C6H5 to C6H11 (the benzene ring was reduced to a cyclohexane ring).<br>(+)-Phenylisopropylmethylamine (PhCH2CHMeNHMe) was prepared in 95% yield as the<br>crude hydrochloride salt from 4 g. ephedrine hydrochloride, 90 cc. acetic acid,<br>4.7 g. 84% H2SO4, and 1 g. palladium wool. M.p. 166-8�, m.p. 182� (from<br>chloroform and ethyl acetate).<br><br>I don't notice any obvious errors in this logic. also, I believe that Pd/C or Pd/BaSO4 would work fine as catalysts. I am assuming that this reaction needs to occur under pressure and with somewhere between 60-90C temperature. </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post68530"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> Ballistic<br> <i>(<span title="The user's title at the time of posting">Stranger</span>)</i><br> <span title="Posting date">11-10-00 14:40</span><br> <span title="Link to this post by using the markup [68530]">No 68530</span><br> </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">Re: Catalytic Hydrogenation......</b> </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> So what you guys are saying is that this rxn produced something but it wasn't meth. All the other rxn of this type<br>did include acetic acid. Would there be something you could<br>substitute for acetic acid that one could produce or acuire<br>without going to a chem store?<br><hr><br>The rain in Maine falls mainly down the drain. </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post68534"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> serodronin<br> <i>(<span title="The user's title at the time of posting">Stranger</span>)</i><br> <span title="Posting date">11-10-00 14:55</span><br> <span title="Link to this post by using the markup [68534]">No 68534</span><br> </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">Re: Catalytic Hydrogenation......</b> </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> they make something, but it ain't meth. just gives you a buzzy headache you wish would go away.<br><br>glacial acetic acid is kept in quantity at photo supply stores. really simple to get, just go in and pay cash. no questions asked. if you're really paranoid or can't find a photo supply store, go to the grocery store and get white vinegar. you can distill it out from there. </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post68550"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> <font color="#FF0033">WizardX</font><br> <i>(<span title="The user's title at the time of posting">Wizard Master</span>)</i><br> <span title="Posting date">11-10-00 15:39</span><br> <span title="Link to this post by using the markup [68550]">No 68550</span><br> </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">Re: Catalytic Hydrogenation......</b> </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> The easiest way to make H2 gas is Aluminium and Sodium hydroxide solution (1M). The H2 gas can then be compressed into a gas cylinder while cooled in ice. </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post68558"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> placebo<br> <i>(<span title="The user's title at the time of posting">irritable and cranky</span>)</i><br> <span title="Posting date">11-10-00 17:08</span><br> <span title="Link to this post by using the markup [68558]">No 68558</span><br> </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">Re: Catalytic Hydrogenation......</b> </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> This is KrZ's write-up called "Mastermind" I believe.<br>I am not sure, but I thought it had been tried and was succeful by others, but I may just have an over-active imagination and a un-natural need to stroke KrZ's ego. I am sure Rhodium would not have put it up on his site if it had no merit and obvious errors. But stranger things have happened! Look at the mole on Stonium's bum. <br><hr><br>Wanna do the rumpy pump? </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post68568"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> terbium<br> <i>(<span title="The user's title at the time of posting">Hive Bee</span>)</i><br> <span title="Posting date">11-10-00 18:18</span><br> <span title="Link to this post by using the markup [68568]">No 68568</span><br> </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">Re: Catalytic Hydrogenation......</b> </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> <blockquote title="Quoted text"><hr><p>I am sure Rhodium would not have put it up on his site if it had no merit and obvious errors.<p><hr></blockquote><p>How about the catalytic hydrogenation of phenylalanine to amphetamine that is on Rhodium's site. Does anybody really think that that works?<br><br><a href="http://rhodium.lycaeum.org/chemistry/phenylalanine.txt" target="_blank" title="Jump to this external site">http://rhodium.lycaeum.org/chemistry/phe<wbr>nylalani<wbr>ne.txt</a><br><br>Another one I like is the rP/I reduction procedure that calls for placing the iodine and rP together in a ball mill so that they will be "thoroughly mixed".<br><br>And then there is the procedure we are discussing here that calls for removing the air from the hydrogenation reactor by "mouth suction". This would be funny if it weren't that some people will actually believe it. </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post68938"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> KrZ<br> <i>(<span title="The user's title at the time of posting">Hallucinogenius</span>)</i><br> <span title="Posting date">11-12-00 17:23</span><br> <span title="Link to this post by using the markup [68938]">No 68938</span><br> </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">Re: Catalytic Hydrogenation......</b> </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> That reaction is an exact duplicate of the reference which someone posted only days before, I will see if I can find it. Mouth suction is a joke for idiot meth cooks, like all those warnings you see about mouth pipetting that are still around today even though it hasn't been done in decades. </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <td align="left" valign="top" class="text_bg"> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post392325"></a><a name="last"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> Organikum<br> <i>(<span title="The user's title at the time of posting">Hive Addict</span>)</i><br> <span title="Posting date">12-23-02 22:40</span><br> <span title="Link to this post by using the markup [392325]">No 392325</span><br> </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">for completeness</b> </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> ok, this is a quite old thread but I want to add something for not misleading bees on search.<br><br>The german <a href="http://l2.espacenet.com/dips/viewer?PN=DE968545&CY=gb&LG=en&DB=EPD" target="_blank" title="Jump to this patent">Patent DE968545</a> by Knoll AG from 1958 states that the by in post <span title="Jump to this post"><a href="../crystal/000068385.html#Post68517">Post 68517</a> <i>(serodronin: "Re: Catalytic Hydrogenation......", Stimulants)</i></span> cited reference <blockquote title="Quoted text"><hr><p>Kindler et al., The Mechanisms of Chemical Reactions. X. Preparation of Phenyl-and Cyclohexylalkylamines by Hydrogenation. Justus Liebigs Ann. Chem., 560, 215-21 (1948); C.A. 43: 1025g (1949).<p><hr></blockquote><p>is wrong as this will not work as described with H2SO4. <br>The patent further describes a ephedrine.HCl reduction with in GAA solved HCl and Pd sponge as catalyst. The catalyst/substrate ratio is insane. The procedure can be modified by using 10%Pd/BaSO4 or 10%Pd/C as catalyst in a much lower ratio and adding small amounts of 70% HClO4 (which has to be diluted in GAA before addition). With this modifications it is a very good yielding synth for clean substrates.<br><br>ORG<br><hr><center><font color="blue"><b>now or never</b></font color="blue"></center> </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> <img src="../forum/images/left_top.gif" border="0" height="12" width="9"></td> <td colspan="7"><a name="Post507994"></a><a name="last"></a></a> </td> <td align="right" valign="top"><img src="../forum/images/right_top.gif" border="0" height="12" width="9"></td> </tr> <tr class="text_bg"> <td rowspan="2"> </td> <td rowspan="2"> </td> <td valign="top" align="center" rowspan="2"> <font color="#FF0033">Rhodium</font><br> <i>(<span title="The user's title at the time of posting">Chief Bee</span>)</i><br> <span title="Posting date">05-18-04 13:05</span><br> <span title="Link to this post by using the markup [507994]">No 507994</span><br> </td> <td rowspan="2"> </td> <td rowspan="2" width="1" class="vert_ruler"> <img src="../forum/images/hr.gif" border="0" width="1" height="1"> </td> <td rowspan="2"> </td> <td class="text_bg" align="left" valign="top"> <b title="The subject of this post">Catalytic Hydrogenation of Ephedrine to Meth</b><br> <i title="This post has been up-rated by the moderators">(Rated as: excellent)</i> </td> <td class="text_bg" align="right" valign="top"> </td> <td> </td> </tr> <tr class="text_bg"> <td colspan="2" valign="top" align="left"> <br> <b>�ber die Darstellung von β-Aryl-alkylaminen</b><br><i>Karl Wilhelm Rosenmund & Erwin Karg</i><br><a href="../rhodium/pdf /ephedrine.hydrogenation.rosenmund.pdf" target="_blank" title="Jump to this external site">Chem. Ber. 75, 1850-1859 (1942)</a> (../rhodium/pdf /ephedrine.hy<wbr>drogenat<wbr>ion.rose<wbr>nmund.pd<wbr>f)<br><br><sub>Mentioned before in:<br><span title="Jump to this post"><a href="../DUMMY">Post 71342</a> <i>(serodronin: "Preparation of B-arylalkylamines", Methods Discourse)</i></span> (Contains english abstract of this article)<br><span title="Jump to this post"><a href="../DUMMY">Post 269642</a> <i>(MethKat: "paladium ingot", Stimulants)</i></span> </sub><br>____ ___ __ _<br><br><b><sub>Studien �ber den Mechanismus chemischer Reaktionen. X.</sub><br>Phenyl- und Cyclohexyl-alkylamine durch Hydrierung</b><br><i>Karl Kindler, Bruno Hedemann, Ernst Sch�rfe</i><br><a href="../rhodium/pdf /ephedrine.hydrogenation.kindler.pdf" target="_blank" title="Jump to this external site">Ann. Chem. 560, 215-221 (1948)</a> (../rhodium/pdf /ephedrine.hy<wbr>drogenat<wbr>ion.kind<wbr>ler.pdf)<wbr><br><br><sub>Mentioned before in:<br><span title="Jump to this post"><a href="../crystal/000068385.html#Post68517">Post 68517</a> <i>(serodronin: "Re: Catalytic Hydrogenation......", Stimulants)</i></span> (Contains english abstract of this article)<br><span title="Jump to this post"><a href="../DUMMY">Post 359515</a> <i>(Chicken: "This refernce", Stimulants)</i></span><br><span title="Jump to this post"><a href="../crystal/000068385.html#Post392325">Post 392325</a> <i>(Organikum: "for completeness", Stimulants)</i></span></sub> <br> <span title="The signature"><hr><sup>The Hive - Clandestine Chemists Without Borders</sup></span> </td> <td> </td> </tr> <tr class="text_bg"> <td align="left" valign="bottom"><img src="../forum/images/left_bottom.gif" border="0" height="12" width="9"></td> <td valign="middle" align="center" colspan="7"> </td> <td align="right" valign="bottom"><img src="../forum/images/right_bottom.gif" border="0" height="12" width="9"></td> </tr> <tr class="page_bg"> <td colspan="9"> </td> </tr> </body> </html>