complet DMT synth :)

brain · Linguist Extraordinaire

I will be happy when you will be helping me with hese synthesis Smile

i have:
1)first stage-decargoxylation of tryptophan

-5g l-tryptophan
-100ml-cycloheksanol
-100ml cycloheksanon
-methanol

the main idea is to mix these substances in proportions : 5g tryptophan, 20-40ml cyclohexanol, 0,3-0,4ml cyclohexanon, 20-50ml methanol - methanol is for makeing the pseudo"inert" atmospher Smile

, than i want to add some H2SO4+IPA after decarboxylation, then tryptamine sulphate will precipate?? then filtrate, wash, basyfied, extracted.

2)methylation
-tryptamine
-HCHO

heat this Smile

3)demethylation
-product from above
-NaBH4
-CH3OH

cool before reduction, the rest of HCHO - will hydrogenate to CH3OH,basyfied[nececery?], than i want to add H2O [CH3OH-will disolwe in water], extract with Et2O, ewaporate Smile

I have it-Im just finding time to do these Smile

brain · Linguist Extraordinaire

L-tryptophan 2x2,5g :

cyclohexanol 100ml :

cyclohexanon 100ml :

me 'decarboxylation' glass (reflux):

HCHO 1l :

from chemicals i have also DAB - for recowering indoles on TLC, methanol, NaBH4

yaya · Thu May 19, 2005 6:11 am

your psudo inert atmosphere is interesting, but why risk it? Go to the wine store and see if you cant find your self a can of spray in wine saver/preservative stuff, I think it's mostly Ar. Or just get some N2.

What is your catalyst? Is it cyclohexANONE or is it a cyclohexENONE? There is a difference and I am wishing to know what happens regardless of which one you have.

see "tryptophan decarboxylation" for more questions and idea for monitoring reaction progress

brain · Linguist Extraordinaire

i will use as catalis cyclohexANONE , my friend done that couple days ago in good yelds, with MeOH addition ... Smile

but i want to try it by my self-and check it Smile

IndoleAmine · Dreamreader Deluxe

Try cyclohexanol as solvent, it is high-boiling. Cyclohexanone as ketone decarbox catalyst might work too, but I seem to remember that you need a a,b-unsaturated ketone (an -ENONe, no -ANONe) for such things..

MeOH would lower reflux temp. to below 100°C I would bet - and you need as high temp. as possible, decarbox. is really endothermic..

Maybe you could try applying vacuum instead inert atmosphere? it would help for better de-gassing, and for removing the evolving CO2 more quickly

(->"LeChatelier principle", A+B<>C+D; addition of more A or B means more of them reacts, continuous removal of C or D means the same..)

brain · Linguist Extraordinaire

and what about (Rhodium) :

IndoleAmine · Dreamreader Deluxe

Sounds indeed like normal, satd. ketones would work well too.

Try it, and report back - then we know for sure.

I remember that numerous experienced bees didn't succeed with tetraline/cyclohexanone, and xylene/acetone was tried without much success too.

But you never know..

brain · Linguist Extraordinaire

i think i will test it tomorrow, how to detect tryptamine (not tlc method) anyone knows? ...if no-i will make tlc , and compare with "test" tlc's ...

IndoleAmine · Dreamreader Deluxe

There are color test reagents for qualitative analysis: Van Urk Reagent can indicate indole compounds, and you can check for presence of amino acids with many other similar tests I bet (don't know any from memory). Fischer's reagent can differentiate between primary, secondary and tertiary amines, if this is of use to you.

Think you get the picture? Very Happy

yaya · Tue May 24, 2005 4:50 am

“my friend done that couple days ago in good yelds”

Oh do tell…any details would be nice……how much, how long, cat./tryp ratio……yield. Do you plan on recycling your solvent after H2O/H2SO4 acidification? How will you separate unreacted tryptaphan?

here is an old post from the hive back in the day...one of the very few dealing with NaBH4/formalin....... thought you might like a look.....even though, if I remember correctly many doubted the authenticity of it.
"
Hi,bees!
SWIM methylated tryptamine and 5meotryptamine with NaBH4 and CH2O aq.
There is description of synthesis:
The 0.8g tryptamine was dissolved in 20ml MeOH and cooled in refregerator(t minus 10C)1-2hours. Flask got from refregerator and dropped 1/10 part of 37% CH2O aq(on 1mole tryptamine take 4moles FORMALDEHYDE),shaked 1 minute and added a few (on the knife top)powder NaBH4(1g borhydride on 1g tryptamine approximatly)and vigorously shaked. When sodium borhydride was dissolved next part of 37% CH2O aq dropped and so on until all CH2O and NaBH4 was conducted to reaction(40min-1.5hours need).The temperature was keep about 5-20C(cooled in refregerator if need). The reaction mix allowed stand at room temperature some hours. Rm was diluted water, MeOH disstilled and product extracted CHCl3. Solvent removed in water bath, specific smell oil(weight 0.9g) yielded. Smoke 50mg its oil produce intense open/close eye visuals, time distortion, empathy and other strong effects. Duration up to 15min. Can anyone repit its synthesis and determine how much Dmt consist in that oil?
Sorry, my english is poor.
"

there go,
Thanks
and good luck

brain · Linguist Extraordinaire

when i will bought 100g of l-tryptophan i will test rest of synthesies ... but now i wont to try decarboxylation like abowe add h2so4 and hill it (first methanol distilled of?) , then add formalin in room temperature (more formaline than needed) than chill it to -10,-15C and add NaBH4, than slowely heated to 5-10C, than room temperature-couple hours...

is it nececery to separate l-tryptophan and tryptamine? if is-i will separate it on TLC (i was talking about it).

btw~i dont hawe time, i hawe hope to test it in this week

yaya · Thu May 26, 2005 4:40 am

“is it nececery to separate l-tryptophan and tryptamine? if is-i will separate it on TLC (i was talking about it).”

Dude………I would highly, highly, highly suggest you perform this reaction with the purest of reagents and fallow the article procedure exactly.

Your going to separate enough for a reaction using tlc?

“i will use as catalis cyclohexANONE , my friend done that couple days ago in good yelds, with MeOH addition ... but i want to try it by my self-and check it

If your friend shared any more specific info please pass it on.

Thanks
Good luck

brain · Linguist Extraordinaire

prankster · Mon Jun 13, 2005 2:16 am

Wow. I salut you for this thread.
I hope you give us a complete DMT write-up.

IPN · Wed Jun 15, 2005 9:32 pm

Swii has 150ml 1-octanol, 10ml methyl ethyl ketone and 15g tryptophan copper chelate at reflux in a 250ml rbf. Swii will reflux for approximately 72h and try to extract the possibly formed tryptamine with chloroform after basifying with NaOH.
Swii also has some old graffiti remover which is 80% NMP. That will be tried next if octanol doesn't give good results.
These are the only high-bp solvents swii has available at the moment. Has anyone tried xylene? Swii remembers reading that it would need very long reflux times and only gives low yields. Is this true?