TIHKAL 6#

[Captain_Mission]

In tihkal #6 shulgin outlines a procedure to transforn the iodine salt of N,N,N-DMT to the chloride salt and it´s demethylation. All the reagents seem easy to obtain and the procedure seems simple when compared to the other demethylation procedures of the book, or any of the DMT synthesis I´ve seen so far. I checked the new and old hive and nobody mentions this method. Can anybody more experient comment on this? If it´s necessary I can post the procedure here.

[Captain_Mission]

OK. I realized my post was a bit vague so I´m going to place a few specific questions. I´ve read the procedure 50 times now and I can´t understand where the demethylation is taking place. I Also wanted to find a way to avoid using picric acid. I really wanted to explore this further because it looks like a very simple and OTC route to DMT: it doesn´t involve any hard-to-get reducing agent like LAH or NaBCNH3 and all the other chems can be either made or easilly found except picric acid. Comments, please.  

[terbium]

This salt was pyrolyzed under hard vacuum
This would be where the demethylation is occurring. The picric acid is just used to make an easily crytallizable material for purification of the DMT, another method of purification such as column chromotagraphy could be used. I didn't see where he gave a yield for this procedure - it must have been pretty poor.

If one doesn't have access to LiAlH4 to reduce the amide then extraction of DMT from Mimosa hostilis or Desmanthus illinoensis root bark is probably the next best method.

[baalchemist]

Go Desmanthus!!!

[Captain_Mission]

What about making the LAH from AlCl3 and LiH? I,ve seen a post in the old hive where someone claimed to have done this following the intructions in rhodium´s page. It sure doesn´t seem very easy, at least with improvised equipment, but it leaves me wondering.

[terbium]

Sure, one could make LiAlH4 from LiH but LiH is not likely to be easier to obtain than LiAlH4.

[pyrotek]

fuckin picric acid is fuckin piss to get/make fuck ya
fuckin if your conderign makin Dmt well fuckin if u cna't make soem smpal p acid your fuced
fuckin

Just Shoot it , think later
were would the WORLD be with out MY 12 gauge

[hest]

Boil salicyl acid in konc. HNO3 for 60min, pour it out on ice and colect the picric acid yeld close to 95%
(if you wonder, the carbox. group doo disapear)

[Captain_Mission]

This is the interesting part of that old board post I mentioned:
 
DJX
unregistered   posted 06-25-1999 12:28 PM           
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I do not know where you can buy metal hydrides, but you can make it.
Heat Elementar Lithium to the mp (181°C).
Then let Hydrogen gas (H2) stream over this now liquid Lithium.
The product is colorless or white salty.
This is Lithiumhydride (LiH).
You can use it to make Lithiumaluminiumhydride better known as LAH.
Combine the LiH with waterfree!!! Aluminiumchloride (AlCl3) an heat.

4 LiH + AlCl3 --> LiAlH4 + LiCl

Then remove the LiCl.

An do not forget: All reactions *MUST* be ablolutly Waterfree !!!

 
timeless
Member   posted 06-26-1999 11:40 AM          
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I made a lot of LAH with LiH and AlCl3.
I used the procedure on rhodiums site and i have to say that it works very well,you only need a lot of ether.
you can make the LAH and the reuction in one pot, yields are about 85-90% for amphetamine from 2pnp. 
 

[phaidon]

And where would one get that lovely salt?  

Laters,

-- phaidon, son of apollon

I scorched the Earth, now what do I do tomorrow?

[terbium]

From the reaction of tryptamine with methyl iodide.