RDXHMX (Stranger)
02-01-02 11:19
No 263880
      DMT syntheses  Bookmark   

does anybody have any experience with the DMT synthesis,
tryptamine+NaCNBH4+CH2O 38%+MeOH+GAA i would like to here from other people what thy think about this DMT route and does it work or not,
i don`t want to fuck`up hard to get and expensive chemimicals
 
 
 
 
    halfapint
(Ubiquitous Precursor Medal Winner)
02-02-02 10:45
No 264239
      Re: DMT syntheses  Bookmark   

Or condensation of indole with DMAE (dimethylaminoethanol) or dimethylaminoethylene?


a half a pints a half a pound a half a world a half a round
demimonde, n. Half world.
 
 
 
 
    RDXHMX
(Stranger)
02-02-02 23:54
No 264553
      Re: DMT syntheses  Bookmark   

indole is almost inpossible to get in my country,tryptamine isn`t,its not controlled and so i would like to try this route,or the one with MeI __>AgCl2pyrolysis,but AgCl 2much more expensive
 
 
 
 
    Rhodium
(Chief Bee)
02-03-02 02:06
No 264588
      Re: DMT syntheses  Bookmark   

I think that if you use the KrZ protocol, everything is going to be just fine for you.
There are literature references on exactly this reaction available in J Med Chem 44(23), 3881 (2001).

KrZ: Tryptamine -> DMT

Tryptamine hydrochloride (10 g, 62.4 mmol) and sodium cyanoborohydride (6.28 g, 100 mmol) in a mixture of methanol (400 mL) and glacial acetic acid (11.76 g, 196 mmol) were cooled to 0C in an ice bath over a steady stream of nitrogen. A solution of 4.20 g formaldehyde (140 mmol, 11.05 mL of 38% Aq. CH2O) in 125 mL of Methanol was added dropwise to the solution over a period of one hour with mild stirring. The flask was stoppered, the reaction allowed to return to room temperature slowly, and allowed to proceed for the next 60 hours. Upon completion the pH was adjusted to 8.0 by the dropwise addition of an aqueous solution of sodium bicarbonate. The mixture was then extracted 4x with 50 mL of ethyl acetate. The combined extracts were washed once with 250mL of brine and dried over MgSO4 (15g) for 15 minutes. The MgSO4 was washed clean with another 75 mL of ethyl acetate. The solvent was reduced to 100 mL on the rotary evaporator. The hot solution was added to a 200mL beaker and covered with plastic wrap which was sealed on with a rubber band. Upon cooling in the freezer overnight, the precipitated DMT was removed by filtration, and dried in the dessicator.

Overall yield: 7.88g, 45 mmol, 67%. The mp is solid, right around 64-67C.
 
 
 
 
    bucockey
(Stranger)
02-03-02 08:18
No 264673
      Re: DMT syntheses  Bookmark   

I have a few questions regarding KRZ's synth.
Number one, (and I have UTFSE) has the lower yeilding version (without the inert environment)of that tech been reproduced (rather - are bee's certain of its reproducability)?
number two: I have seen NaCNBH4 and NaCNBH3 cited interchangably throughout this site - I assume that the - NaCNBH3 is what is to be used for the synth (correct me if Im wrong) swib is wondering if he was able to acquire NaCNBH4 would  he be able to treat it with something (he's pretty certain he saw a post describing a method but cant remember the # off hand) and convert it to NaCNBH3? (and he is also quite aware to keep the stuff dry)
and question number three is for Rhodium directly: what do you think about the indolyl-ethyl-bromide route with tryptophol as suggested by Lilenthol (says its an easy otc route to elfland)? (post # 7781 and 197106 - sorry, I cant figure out how to make those links to other posts work without erasing my message - this is actually the third time Ive typed this post!)
 
 
 
 
    RDXHMX
(Stranger)
02-03-02 09:16
No 264686
      Re: DMT syntheses  Bookmark   

thank you rhodium,this is what i was looking for.
 
 
 
 
    terbium
(Old P2P Cook)
02-03-02 10:49
No 264702
      Re: DMT syntheses  Bookmark   

I have seen NaCNBH4 and NaCNBH3 cited interchangably throughout this site - I assume that the - NaCNBH3 is what is to be used for the synth (correct me if Im wrong) swib is wondering if he was able to acquire NaCNBH4 would
The formula of sodium cyanoborohydride is NaBH3CN (or NaCNBH3 if you prefer). You will not be able to acquire NaCNBH4 (or NaBH4CN) because it does not exist.
 
 
 
 
    Rhodium
(Chief Bee)
02-03-02 16:27
No 264784
      Re: DMT syntheses  Bookmark   

I think the tryptophol route sounds really good, it is too bad that there ain't noone here who has tried it yet - only other chemists in 50 year old journals.
 
 
 
 
    dely72
(Newbee)
02-05-02 10:43
No 265548
      Re: DMT syntheses  Bookmark   

I have one question as well. instead of using nitrogen to produce an inert atmosphere could you simply use helium? I was reading an MDA synth on rhodiums site using sodium cyano, and it said that you could take a baloon filled with nitrogen and simply blow out the oxygen in the flask and then place the baloon over one of the necks of the flask (and tape it down of course). Could You create a poor mans inert atmosphere by simply using a helium baloon? Perhaps with lower yeilds but hey, they will probably be better than the 33% yeilds under normal atmospheric conditions.
 
 
 
 
    yellium
(Hive Addict)
02-05-02 11:27
No 265557
      Re: DMT syntheses  Bookmark   

Helium is lighter than air. Argon (used for welding) will do.
 
 
 
 
    RDXHMX
(Stranger)
02-06-02 01:55
No 265882
      Re: DMT syntheses  Bookmark   

about tryptophol,is it true you have to use Me2NH anhydrous (gasform) for the synthesis or is there an other way and 2nd does some one has a good ref. for homebrewing AgCl2,i will let you all know how the reaction went whith NaCNBH3 next coming weeks.keep up the good work !!!
 
 
 
 
    Lilienthal
(Moderator)
02-06-02 06:20
No 265946
      Re: DMT syntheses  Bookmark   

Dialkylamine in methanol at RT should be working fine from what I've heard - even if the published procedures for this synthesis are old and low-yielding.
 
 
 
 
    cilliersb
(Hive Bee)
02-07-02 03:06
No 266407
      Re: DMT syntheses  Bookmark   

The whole NaBH3CN synth looks fine except for one thing.

" formaldehyde (140 mmol, 11.05 mL of 38% Aq. CH2O)"

Correct me if I'm wrong, but the water in 38%Aq CH2O will destroy your Boro. Should you not try to rather dissolve CH2O in Methanol instead of using 38%Aq?

Just a though you know, since we're all so concerned with the inert atmosphere to exclude water and all.
 
 
 
 
    Rhodium
(Chief Bee)
02-07-02 05:38
No 266433
      Re: DMT syntheses  Bookmark   

Aqueous formaldehyde is all right to use with sodium cyanoborohydride, the small amount of water will not hydrolyze the hydride faster than the aldehyde/tryptamine imine is reduced. But, as you guess, an alcoholic solution of formaldehyde would be better to use in this instance. To make a such solution, depolymerize paraformaldehyde in a flask and distill the firmed gas into a chilled container with the alcohol.
 
 
 
 
    foxy2
(Distinctive Doe)
02-07-02 15:23
No 266658
      Re: DMT syntheses  Bookmark   

"the small amount of water"

Thats the first time I have heard of 62% water being a "small amount". 
tongue

I'm not saying it won't work.

Fully Informed Jury! (http://www.fija.org/)
 
 
 
 
    sunlight
(Pioneer Researcher)
02-07-02 18:26
No 266713
      Re: DMT syntheses  Bookmark   

Do you know any reference of reductive amination of IAA with dimethylamine or diethylamine ? It could be a relative easy way to make DMT, it has been mentioned in the Hive, but without references.
 
 
 
 
    terbium
(Old P2P Cook)
02-07-02 20:02
No 266735
      Re: DMT syntheses  Bookmark   

Do you know any reference of reductive amination of IAA with dimethylamine or diethylamine ?
Ahh, IAA = indoleacetaldehyde? When I see the abbreviation IAA I usually think indoleacetic acid.
 
 
 
 
    sunlight
(Pioneer Researcher)
02-08-02 07:13
No 266922
      Re: DMT syntheses  Bookmark   

Sorry, I want to mean indol 3 acetaldehyde with IAA, but yes, it is used for the acetic acid, you're right,
 
 
 
 
    meme
(Hive Bee)
02-22-02 11:58
No 272134
      Re: DMT syntheses  Bookmark   

Poster: Rhodium
Subject: Re: DMT syntheses

"I think the tryptophol route sounds really good, it is too bad that there ain't noone here who has tried it yet - only other chemists in 50 year old journals.  "

Go ahead and make me all horny, Rh

 
blush

Solve et Coagula.