Rhodium
(Chief Bee) 03-22-04 08:51 No 496649 |
Sodium triacetoxyborohydride | |||||||
Sodium triacetoxyborohydride is very likely to work. UTFSE here and at rhodium.ws to find out general procedures and preparation of the reagent. The Hive - Clandestine Chemists Without Borders |
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tryin (Stranger) 03-22-04 20:29 No 496781 |
Thank you very much Rhodium. | |||||||
Thank you very much Rhodium. I have a question about when Phikal says he used 4.4 g 3,4-methylenedioxyphenylacetone (MDP-2-P). Is this the same as 4.4 mL? Also I can only find info on O-methylhydroxylamine hydrochloride but Phikal uses N-methylhydroxylamine hydrochloride. What is the difference? |
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Rhodium (Chief Bee) 03-23-04 01:32 No 496820 |
FLEA precursors | |||||||
I have a question about when Phikal says he used 4.4 g 3,4-methylenedioxyphenylacetone (MDP-2-P). Is this the same as 4.4 mL? You really should weigh out your reagents. Also I can only find info on O-methylhydroxylamine hydrochloride but Phikal uses N-methylhydroxylamine hydrochloride. What is the difference? The difference is where the methyl group is attached. The compounds are very different. NH2O-CH3 (O-methyl) CH3-NH2OH (N-methyl) The Hive - Clandestine Chemists Without Borders |
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tryin (Stranger) 03-24-04 14:01 No 497093 |
Again I thank you for helping me. | |||||||
Again I thank you for helping me. I'm sorry if my questions are stupid. But that's what the newbee forums are for, right? I have another question. Phikal states:"The reaction appeared to have stopped after a day or two, so all was poured into 500 mL H2O, acidified with HCl, and washed with 2x75 mL CH2Cl2. The addition of base brought the pH >9, and this was then extracted with 3x75 mL CH2Cl2" What is he using for a base to bring the pH >9? Would sodium carbonate work? Also, what would be the best way to recrystallize? |
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Rhodium (Chief Bee) 03-24-04 15:34 No 497105 |
Acid/Base Extraction & Recrystallization | |||||||
I have another question. Phikal states:"The reaction appeared to have stopped after a day or two, so all was poured into 500 mL H2O, acidified with HCl, and washed with 2x75 mL CH2Cl2. The addition of base brought the pH >9, and this was then extracted with 3x75 mL CH2Cl2" What is he using for a base to bring the pH >9? Would sodium carbonate work? He is likely using 10-20% sodium hydroxide, for a more in-depth discussion see Post 496626 (fanofshulgin: "This is real easy to answer.", Newbee Forum) Also, what would be the best way to recrystallize? It depends on too many factors to answer in a post like this. Read up on it in the documents below: Recrystallization Basics (../rhodium /equipm Recrystallization Technique (../rhodium /equipm The Hive - Clandestine Chemists Without Borders |
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tryin (Stranger) 08-12-04 22:44 No 525194 |
Thank you for answering my posts Rhodium. | |||||||
Thank you for answering my posts Rhodium. Some other questions I have are these; Shulgin writes "The free-base product from these preparations was distilled at 110-120 °C at 0.2 mm/Hg to give the N-hydroxy-N-methyl product as a white oil." Can your average 3cfm robinair vacuum pump pull this over at this temperature? If not, which I suspect, how do you determine at which temp. the N-hydroxy-N-methyl product white oil will come over with a different mm/Hg? |
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Rhodium (Chief Bee) 08-13-04 10:58 No 525286 |
See the Nomograph at my page | |||||||
how do you determine at which temp. the N-hydroxy-N-methyl product white oil will come over with a different mmHg? See my Nomograph for Calculation of Boiling Points Under Vacuum (../rhodium /equipm The Hive - Clandestine Chemists Without Borders |
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tryin (Stranger) 08-14-04 13:46 No 525426 |
Thank you, thank you I guess I need to use the | |||||||
Thank you, thank you I guess I need to use the search engine on Rhodium more. There are a lot of good things I haven't even began to look at. |
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tryin (Stranger) 08-19-04 07:10 No 526299 |
According to the Sodium triacetoxyborohydride... | |||||||
According to the Sodium triacetoxyborohydride MSDS it needs to be stored in closed system under dry nitrogen gas. Is this absolutely neccessary? My goal in starting this thread is about whether a home chemist could safely (with less toxic chemicals) synth FLEA? It seems to me that it could be done if there was a way around the Sodium triacetoxyborohydride. But I don't think that there is so it will have to remain in my opinion, just a dream. If anyone can help me realize this dream with less toxicity please let me know. |
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Kinetic (Hive Bee) 08-19-04 08:32 No 526304 |
FLEA | |||||||
Why FLEA? The only reason I can think that someone would want to make an N-hydroxy analogue of a controlled substance would be bypass the legal restrictions on the parent compound. I take it from the style of your questions you aren't an experienced chemist. There is nothing wrong with that, but you should be aware that even very experienced chemists with well equipped labs will find it extremely difficult - if not impossible - to synthesise an N-hydroxy analogue of any amphetamine derivative without risking some decomposition to the parent amphetamine. Compounding the situation in your case is the requirement of MDP2P, which you must first make. The synthesis of this alone is likely to be sufficient to secure a conviction based on a conspiracy charge. Do not attempt to make FLEA, or any other N-hydroxy PEA or amphetamine analogue unless you realise that the consequences of doing so are likely to be no better than for making the parent drug intentionally. Here is part of the extensions and commentary from PiHKAL#114 MDOH (http://www.erowid.org/library/books_onl
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tryin (Stranger) 08-20-04 12:21 No 526500 |
that is the reason | |||||||
Why FLEA? The only reason I can think that someone would want to make an N-hydroxy analogue of a controlled substance would be bypass the legal restrictions on the parent compound. Well you caught me. This is the reason I am interested in the compound. I figured that if I got past the MDP2P step that I would be home free legally speaking. In the back of my mind I never really can convince myself though. Thanks for pointing out the risk more clearly. However, I do have a few questions. 1. How can FLEA be converted to MDMA accidently, since a hydroxy is being used? 2. Also is there a different chemical other than Sodium triacetoxyborohydride that could be used? (this is just for knowledge sake) 3. Is there any legal substances in the U.S. that are worthwhile to look into? ( I understand if no reply is made to this question because then that is what will become illegal next) |
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Barium (Heavyweight Chempion(eer)) 08-20-04 15:20 No 526523 |
Is there any legal substances in the U.S. | |||||||
Is there any legal substances in the U.S. that are worthwhile to look into? Ever heard of the "analogue act"? If not look it up and read it. Pretty much anything with a beta-phenylethylamine skeleton is covered with that law, if it is made for consumption in any way. Forget the foolish idea behind the RC's. That era is over. How can FLEA be converted to MDMA accidently, since a hydroxy is being used? There are several ways. Reduction for example. Also is there a different chemical other than Sodium triacetoxyborohydride that could be used A cyanoborohydride or borane could be used too. A triacetoxyborohydride beats any of them by a mile whan it comes to handling issues. UTFSE for sodium triacetoxyborohydride. Severe Aztecoholic and President of Sooty's fanclub - Sooty for President!! |
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Kinetic (Hive Bee) 08-20-04 15:31 No 526524 |
Analogues: a STAB in the dark | |||||||
Edit: This was posted before reading Barium's reply. The reason you have a problem with MDMA formation is because the N-OH group is far less stable than a typical C-OH group (i.e. an alcohol). N-OH is readily reduced to N-H by a large number of reducing agents, and possibly by other means (excessive heating, for example). The N-OH group is so readily reduced to the amine that plain hydroxylamine is often recommended for the synthesis of substituted amphetamines; most reducing agents will give nothing but the amphetamine when performing a reductive amination of a phenylacetone with hydroxylamine. With the more specific reagents such as sodium cyanoborohydride you can halt much of the reaction at the N-OH stage - but, as I said above, there will always be the chance that you have reduced some to the amine. Further, you have no way of knowing, and you cannot take for granted the stability of the product even after the reaction is finished. It may decompose during workup, or during distillation. I want you to be sure of the potential risk you are taking, so I will quote from obia's post Post 324207 (obia: "UK analogues", Law and Order). I hope you can appreciate the relevance of the following:
To answer your next question, sodium triacetoxyborohydride (STAB) can be readily made from not-particularly-toxic sodium borohydride and acetic acid, see Post 439071 (Barium: "Prep of Sodium Triacetoxyborohydride", Novel Discourse). But the suggestion - even by Rhodium - that it is very likely to selectively reduce to the N-hydroxylamine does not mean that it cannot fail. Other reagents that may work are plain sodium borohydride under controlled conditions (e.g. very low temperatures; Shulgin N-methylates MDOH to FLEA with formaldehyde 'at dry ice temperatures'). Borane (BH3, made from sodium borohydride) is a selective reagent and may work, as may the perfluoro analogue of STAB, which can probably be made using trifluoroacetic acid instead of acetic acid in Barium's procedure. Molecule: MDMA and FLEA ("c1c(ccc2c1OCO2)CC(C)NC.c1c(ccc2c1OCO2) Molecule: J (BDB) and Methyl-J (MBDB) ("c1c(ccc2c1OCO2)CC(CC)N.c1c(ccc2c1OCO2) Molecule: Methylenedioxyaminoindane and methylenedioxyaminotetralin ("c1c3c(cc2c1OCO2)CC(C3)N.c1c3c(cc2c1OCO Molecule: 2C-N and DON ("c1(c(cc(c(c1)[N+]([O-])=O)OC)CCN)OC.c1 Molecule: BO-something and Nichols' dragonfly ("c1(c(cc(cc1)OC)C(CN)OC)OC.c12c(c3c(cc1 For the last picture, the BOX analogue has yet to be named as BOH is already taken. It, along with the dragonfly molecule, can be substituted in para- to the aminoethyl or propyl chain with a variety of atoms. Related reading: AET (http://www.erowid.org/library/books_onl J (BDB) (http://www.erowid.org/library/books_onl Methyl-J (MBDB) (http://www.erowid.org/library/books_onl DON (http://www.erowid.org/library/books_onl IAP (../rhodium /iap.ht Methylenedioxyaminoindanes and tetralins (../rhodium/pdf /nichols/nich Nichols' dragonfly (../rhodium/pdf /nichols/nich Good luck. |
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