• N&PD Moderators: Skorpio

cyrstal growing

My answer for the moment:

"Crystal and molecular structure of (N,N)-dimethyltryptamine."
Falkenberg, Goran.
Acta Crystallographica, Section B: Structural Crystallography and Crystal Chemistry 1972, 28(10), p.3075

Abstract

The hallucinogenic indolealkyl-amine, N,N-dimethyltryptamine, crystallizes in 2 modifications having the same monoclinic space group, P21/a and P21/c (z = 8 ). For the latter, which has 2 mols. in the asymmetric unit, data were collected on an automatic diffractometer. Unit-cell dimensions are a 12.99, b 12.08, c 18.38 .ANG., and b 127.85°. The structure was detd. by the symbolic-addn. procedure and refined by the method of full-matrix least squares to R = 0.048 for 2080 obsd. reflections. The mol. structures of the 2 mols. are almost identical. The indole nuclei are planar, and the ethylamine side chain is almost fully extended (torsion angle t = 176 and 188° and mols. A and B, resp.) and lies near a plane which is approx. perpendicular to that of the indole (t = 102 and 90°). Relatively strong N-H...N hydrogen bonds join A mols. (2.92 .ANG.) and B mols. (2.89 .ANG.) sep. in 2 different helically fashioned H-bonding systems around screw axes.

The abstract is not really insightful, so I selected some parts from the publication to (hopefully) clear the issue:

Of the halides of DMT good crystals could only be obtained for the bromide.

(N,N)-Dimethyltryptamine hydrobromide
DMT. HBr:

Transparent light-yellow prisms

Orthorhombic
...which looks like this: http://en.wikipedia.org/wiki/Orthorhombic Already quite close to the Erowid-oic, don't ya think? But the crystals in the pic ain't light-yellow. Ummm... :\

(N,N)-Dimethyltryptamine
DMT (free base!)

Transparent colourless hexagonal prisms

Monoclinic
..which looks like this: http://en.wikipedia.org/wiki/Monoclinic Hexagonal prisms are exactly what we were looking for, or not?

A different publications gives the crystal habit for the free base as "Transparent acicular", 'acicular' being 'Needle-like, slender and/or tapered' (Acta Cryst 1968, B24, p.882), so very much like described here before.

I still doubt that the Erowid-picture shows DMT-freebase. The compound is said to be hygroscopic, which wouldn't render the depicted crystals looking like glass... what they actually do on the foto.

Peace! Murphy
 
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didn't you have that idea a little while ago. Get on that shit already. Might be a sweet way to make ultra pure DMT from dirty DMT.

experimentation needed
 
i havnt had any bark for a while!!!! i did infact have that idea a lonnnnggg time ago. its been since march since ive had any deemsters!

on its way tho :D there will be many many many experiments
 
no, you can't. you will lose too much material due to decomposition. application of a good vacuum pump (lile FnB said) and a sublimation finger are advised. The former costs just some thousand $, no real prob... ;)
 
...what could help (maybe) is the use of protection gas during destillation. This saves product that would otherwise be lost due to oxidation.

Easily available are CO2 and N2, the latter one to be preferred.

Edit: I think I made a mistake with my last post... boiling point of DMT is indeed low enough to make it destillable at atmospheric pressure; so, no need for high vacuum. But decomposition is still an issue IMO. What else could be tried is sublimation! Was this ever mentioned?
 
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Sublimation:

(german) Wiki lists DMT's melting point with 44,6–46,8 °C, and the boiling point being 60–80 °C.
I think that sublimation could be achieved easily, lets say with extern heating of ca. 95 °C and a cooling temperature below 20 °C, but that's not problematic. Light vacuum would be helpful, like from an aspirator

Murphy
 
why wouldn't it work if you just heat it up and gather the DMT along some glass dome (if you allow vaporized DMT to sit spinning for instance in a lightbulb some very fine crystalline deposits will build up on the side).

Theoretically if the impurities are low enough you could get just the DMT to go airborne, couldn't you?
 
Yeah, but I fear that the yield won't be great if some measurements aren't taken. But it would work, no prob...
 
upload it to a hosting site then bracket the link with
tags
 
...naaaah! The boiling point for DMT that I cited from Wiki is complete bullshit. One needs indeed a vacuum pump. Period.
 
Why do you need a vacuum pump if DMT boils into vapour quite readily if you are smoking it in a glass pipe? I really need not mention that you don't need a vacuum to do this. It's not that dissimilar from heating it in a boiling flask in a distillation setup. Admittedly, some of the DMT would crystallise in the condenser, but you could easily recover it by running a NP solvent through it, hexane, heptane, ether, et al.
I suppose doing it under reduced pressure lowers the probability of decomposition, though. Doing it in inert gas (say, N2, or argon) would be a good idea.
 
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I think you won't see a neat destillation 'cause nearly all material will condense too early. Also, decomposition is much increased when applying the boiling temperature at normal pressure. Vacuum is therefore strongly recommended.

- Murphy
 
Word has it that this D freebase crystal was about the size of a quarter. Although it may appear to be yellow, it was completely colorless. The filter paper i rests on, which also appears yellow in the pic, is a pure white.

resized image:
NSFW:
deemsmjr6.jpg


hi-res version. warning: huge
NSFW:
deemwg5.jpg
 
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Dude. Cool picture, but please, make it smaller! I suggest a hosting service that has a thumbnail feature.
 
^ok, but im adding a smaller version instead of replacing the big version. the reason i posted such a big pic is so people could see the details. but youre right it is perhaps too big for many.
 
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