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dextro
(Stranger) 07-20-04 12:58 No 520453 |
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the correct road to amphetamine | ||||||
hi bees ! after spending several days (and nights) with TFSE swid brought back 4 methods from the jungle of routes and methods: 1.)Raney/Urushibara (looks good on the paper) 2.)LAH (seems to be not state of the art) 3.)Al/Hg (poisonous, but wtf...) 4.)Pd/C-GAA-HC00NH4, direct from the p2np (doubtfuly) NaBH4 is not available, overhead stirrer is not the problem. But swid can`t try each route, he only wants to find a confidential bee which can say: "this is the right way for a newbee" the rest of the way home can swid then walk alone. hope there is an answer possible without flaming thx, dex |
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dextro (Newbee) 09-04-04 07:30 No 529547 |
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o.k. after weeks of research swim will try the | ||||||
o.k. after weeks of research swim will try the LAH method. now he has to decide to work with THF or ether. after reaction and workup is done, the freebase is dissolved in THF, is it possible to drip H2SO4 in the THF to make the salt or must the THF distilled off before? thx |
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java (Hive Addict) 09-04-04 11:40 No 529566 |
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Road to Amphetamine..... | ||||||
Read here and get your answer.... Post 459611 (Rhodium: "Reduction of Phenylalanine to Phenylalaninol", Stimulants) Post 459300 (tpower9s2003: "DL-Phenylalanine--->PEA--->Dl-amp Post 516647 (java: "Phenylalanine to amphetamine continuation.....", Serious Chemistry) It is better to die on your feet than to live on your knees....... -Emiliano Zapata- |
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Lestat (Hive Bee) 09-04-04 12:35 No 529573 |
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If you aren't used to working with LiAlH4,... | ||||||
If you aren't used to working with LiAlH4, then I REALLY wouldn't use it as my first cook, it is extremely pyrophoric, and with shitloads of THF/ether around, pyrophoric materials are generally a bad thing ![]() I would bee worried about your safety if you were to try the LAH method, I haven't worked with it myself, but I have seen what it is like, and it is fucking scary! Non omnis moriar, tenebris é clarior |
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dextro (Newbee) 09-04-04 16:30 No 529547 |
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o.k. after weeks of research swim will try the | ||||||
o.k. after weeks of research swim will try the LAH method. now he has to decide to work with THF or ether. after reaction and workup is done, the freebase is dissolved in THF, is it possible to drip H2SO4 in the THF to make the salt or must the THF distilled off before? thx |
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java (Hive Addict) 09-04-04 20:40 No 529566 |
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Road to Amphetamine..... | ||||||
Read here and get your answer.... Post 459611 (Rhodium: "Reduction of Phenylalanine to Phenylalaninol", Stimulants) Post 459300 (tpower9s2003: "DL-Phenylalanine--->PEA--->Dl-amp Post 516647 (java: "Phenylalanine to amphetamine continuation.....", Serious Chemistry) It is better to die on your feet than to live on your knees....... -Emiliano Zapata- |
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Lestat (Hive Bee) 09-04-04 21:35 No 529573 |
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If you aren't used to working with LiAlH4,... | ||||||
If you aren't used to working with LiAlH4, then I REALLY wouldn't use it as my first cook, it is extremely pyrophoric, and with shitloads of THF/ether around, pyrophoric materials are generally a bad thing ![]() I would bee worried about your safety if you were to try the LAH method, I haven't worked with it myself, but I have seen what it is like, and it is fucking scary! Non omnis moriar, tenebris é clarior |
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dextro (Newbee) 09-10-04 06:31 No 530633 |
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swims route is: start with p2np, then red. | ||||||
swims route is: start with p2np, then red. via LAH in dried THF. TFSE found nothing about refluxing time and temp. any suggestions for him? |
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dextro (Newbee) 09-11-04 07:02 No 530845 |
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the addition of the THF/p2np solution to the... | ||||||
the addition of the THF/p2np solution to the LAH/THF solution takes 2 hours. then refluxing for additional 6 hours ???? is this o.k. or too long? |
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Rhodium (Chief Bee) 09-12-04 09:14 No 531016 |
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LAH reflux times | ||||||
Definitely not too long - you can even reflux for 12-24 hours with no ill effects. The Hive - Clandestine Chemists Without Borders |
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dextro (Newbee) 09-15-04 10:05 No 531478 |
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first reaction is done | ||||||
9,5 g LAH in 250ml dried THF and 13,1 g p2np in 100ml dried THF are refluxed for 6 hours. everything fine so far. cooled to RT, then 9,5ml Water are added dropwise to kill remaining LAH. But when the first drop hits the surface of the LAH the solution solidified at this point. result: after the complete addition of the water, the whole solution in the flask solidified to a foamy, bubbling mass, which was impossible to stir. ![]() thought swid has already fucked up now, but proceeded with the addition of 9,5ml 15%NaOH and the additional 50ml THF. > shaked the flask like hell and the whole thing liquified again. additional 28,5ml water but there was no fizzing, SO THIS WAS NONSENSE? but swid read it so. THF was distilled of by vacu. gave me 10ml golden oil, but the smell of this was not as expected (not this typical amine like amphe. smell). WAT IS THE RIGHT SMELL AT THIS POINT? dissolved this in same ammount toluene (bad idea) next time swid will try it with IPA or Ether. but i wanted to do a water wash of the oil (REDUNDANTLY ?), for this reason swid decided for toluol ![]() then 95% H2SO4 was added dropwise. IS IT BETTER TO DISSOLVE THE ACID IN ETHANOL OR IPA 50:50 OR SO? after a little fizzing a white mass formed in the toluene, next drop, same result. white mass was filtered off. again H2SO4, filtered again till no more white is build after addition of acid. after drying swid received ca. 3g. snorted 30mg, not so bad. BUT HELP IS NEEDED at some points (where the letters are BIG) so dex is waiting for some helpful advice. thx again |
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WizardX (Wizard Master) 09-16-04 03:12 No 531596 |
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lithium aluminum hydride | ||||||
Dextro: Have a look at this! PREPARATION OF ENANTIOMERICALLY PURE a-N,N-DIBENZYLAMINO ALDEHYDES: S-2-(N,N-DIBENZYLAMINO)-3-PHENYLPROPANAL http://www.orgsyn.org/orgsyn/prep.asp?pr ![]() Hydrogenation of the aldehyde on the S-2-(N,N-DIBENZYLAMINO)-3-PHENYLPROPANAL Now, removing the N,N-DIBENZYL to aford the -NH2 is a tough one. Maybe using CH3I instead of benzyl bromide in part "A" will give the N,N-DIMETHYLAMINO ?? Another possiblity is to reduce the end product of "B" with HI/P to the S-2-(N,N-DIBENZYLAMINO) amphetamine. Since the amino on the S-2-(N,N-DIBENZYLAMINO) is protected then cyclozation is eliminated. |
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WizardX (Wizard Master) 09-16-04 12:12 No 531596 |
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lithium aluminum hydride | ||||||
Dextro: Have a look at this! PREPARATION OF ENANTIOMERICALLY PURE a-N,N-DIBENZYLAMINO ALDEHYDES: S-2-(N,N-DIBENZYLAMINO)-3-PHENYLPROPANAL http://www.orgsyn.org/orgsyn/prep.asp?pr ![]() Hydrogenation of the aldehyde on the S-2-(N,N-DIBENZYLAMINO)-3-PHENYLPROPANAL Now, removing the N,N-DIBENZYL to aford the -NH2 is a tough one. Maybe using CH3I instead of benzyl bromide in part "A" will give the N,N-DIMETHYLAMINO ?? Another possiblity is to reduce the end product of "B" with HI/P to the S-2-(N,N-DIBENZYLAMINO) amphetamine. Since the amino on the S-2-(N,N-DIBENZYLAMINO) is protected then cyclozation is eliminated. |
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dextro (Newbee) 09-18-04 12:03 No 531964 |
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did another rxn with ether and this way it is... | ||||||
did another rxn with ether and this way it is much easyer and faster with more yield, cause the solvent must not distilled off. dripped h2so direkt in the ether/amin solution and saw a nice snow storm. thats the way. PLEASE: can someone discribe the typ. smell of the freebase oil ? swim thougt it was like flowers but the feebase what he dreamed smells not like flowers. hm ? |
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WizardX (Wizard Master) 09-19-04 06:36 No 532094 |
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amphetamine oil | ||||||
P2NP, C6H5CH2CH(-NO2)-CH3, reduced to amphetamine with LAH. Freebase amphetamine oil has a amine odour (fishy) with a acrid burning taste. Test using Marquis Reagent Amphetamine: orange => brown (blue) Methamphetamine: orange => brown (blue) Ephedrine: yellow-yellow brown (purple) Phenmetrazine: green (blue) Add 9 mls of concentrated sulphuric acid and 1 ml of 40 % formaldehyde solution. OR Add 10 mls of concentrated sulphuric acid and 10 drops of 40 % formaldehyde solution. The colour takes about 15-30 minutes at room temperature to develop. |
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wareami (Hive Addict) 09-19-04 07:35 No 532099 |
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20,000 leagues under the see... | ||||||
WizardX: I could be wrong...but you may want to double check those ratios. I just crossreferenced using the CRC and that didn't help as I think it refers to 100% formaldehyde solution since no %age was given. So I googled and came up with shulgin's ratio His gives 2 drops of 40% formaldehyde and 3 milliliters of concentrated sulfuric acid for marquis reagent. All the references I've seen converting drops to ml= 18-20drops per 1ml. Does that sound right? My personal measures also came up with 20drops exactly per 1ml. Maybe my dropper is smaller than yours ![]() ![]() Even if shulgins is inaccurate...the two example ratios you provided don't look right to me. Making the second one you provided 10drops more acidic. Again I could be wrong with the drops. http://www.cognitiveliberty.org/shulgin/ You Laugh at me because I'm different I laugh at you because you look the same |
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Ascension (Newbee) 09-19-04 13:50 No 532146 |
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Shulgin says the original testing agent was 2... | ||||||
Shulgin says the original testing agent was 2 drops 40% formaldehyde and 3 mls of sulfuric acid but this was the original procedure from 1896. Im sure its been refined a bit since then. Your an individual just like everyone else. |
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WizardX (Wizard Master) 09-20-04 06:49 No 532279 |
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They both work! | ||||||
Wareami: Both shulgin's ratio and mine are correct. They both work. The 2 drops of 40% formaldehyde and 3 milliliters of concentrated sulfuric acid ratio will maybe give a faster colour development? A lab pipette drop is approx 1/10 of a ml. |
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wareami (Hive Addict) 09-20-04 16:14 No 532329 |
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Pipettes Drops and Milliliters | ||||||
Dextro and Bees: I realize this deals more with nonmenclature than the topic at hand. So please forgive the intrusion and hijacking of this thread. WizardX: Cool deal WizardX! Thank you for the clarification. I also noticed that my pipettes dropped more liquid per drop than an ordinary household eyedropper. I guess these type discrepencies lend themselves to inconsistancy between clandestine kitchen/household chemistry and real life lab professional chemistry. Believe it or not...depending on the procedure, this can spell the difference between success and failure where accuracy is a must. As much I felt I was being too anal and/or picky in the above post. (in other words "I wasn't trying to get the DROP on Ya" ![]() ![]() I also knew that your expertise in labwork would help us all arrive at an understanding to diminish the margin to err in all areas...not just this one. Thank You! And thank you as well for describing what may be encountered in more/less concentrate marquis solution. For reagants used as organic indicators, the importance is that the color shows. Unless in extreme "weaker/stronger" marquis solution, "weaker/stronger"=time for color to appear =hue/tint of color indication Now Ibee is more inclined to make a note of the "drop" source whenever he uses drops in write-ups from now on. ie...eyedropper, pipette, blood...sweat...tears...Mr.Johnso......e ![]() Thanx again! http://www.peteducation.com/category_sum Also...see http://www.newton.dep.anl.gov/askasci/ch Looky what I found!(*see pipetters below*)
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