DMT recristallization

[fabio88ct]

Hi guys.
SWIM is very interested to STB. But in this tek there are two cycles of freezing cristallization for a pure product. If Swim roto-evaporates al NPS (petroleum ether), re-dissolve the yellow crystal with warm polar solvent (acetic acic or acetone? some advices?), add petroleum ether drop by drop until the solution becomes milky, cool the solution in a ice bath for a couple of hours and filter the crystal with a vacuum buchner?
What do you think? SWIM use this tek so many times (for other alkaoids) and, based on his personal experiences, thinks it can work.

 

[benzyme]

if you do that, you're deriving a water-soluble salt. is that what you want to end up with?

 

[fabio88ct]

A water soluble salt of dmt? not a freebase?
Swim's goal is to find a faster method for crystallize and ri-crystallize a good product in a couple of hours. Do you think it's possible?
Even if dmt become a water soluble salt, it can not be purified in this form?

 

[pitubo]

SWIM use this tek so many times (for other alkaoids) and, based on his personal experiences, thinks it can work.

I'm curious, what other alkaloids did you extract this way? What polar solvent did you use in those cases to redissolve the crude extracts into and add petroleum ether to in erder to force precipitation of crystals?

 

[1ce]

SWIM use this tek so many times (for other alkaoids) and, based on his personal experiences, thinks it can work.

I'm curious, what other alkaloids did you extract this way? What polar solvent did you use in those cases to redissolve the crude extracts into and add petroleum ether to in erder to force precipitation of crystals?

I'm a little curious about this too. Faster crystals aren't necesarily better crystals.

 

[benzyme]

A water soluble salt of dmt? not a freebase?
Swim's goal is to find a faster method for crystallize and ri-crystallize a good product in a couple of hours. Do you think it's possible?
Even if dmt become a water soluble salt, it can not be purified in this form?

you add acid to the solution, you get a salt, not free base. you can purify the salt with cold pet ether

 

[fabio88ct]

SWIM use this tek so many times (for other alkaoids) and, based on his personal experiences, thinks it can work.

I'm curious, what other alkaloids did you extract this way? What polar solvent did you use in those cases to redissolve the crude extracts into and add petroleum ether to in erder to force precipitation of crystals?

I'm a little curious about this too. Faster crystals aren't necesarily better crystals.

I study chemistry at university and my professor used this technique many times to purify crystals. I used this tek so many times for purify my crude roto-evaporate caffeine crystal (with warm/hot acetone and pet ether drop by drop) and i used too for ricrystallization of capsaicine and piperine (but i dont remeber if i used the same solvents). I know also that faster crystal aren't necesarily better, but my pourpose is to purify faster my solution and, for the final product, use a slow crystallization.

 

[fabio88ct]

A water soluble salt of dmt? not a freebase?
Swim's goal is to find a faster method for crystallize and ri-crystallize a good product in a couple of hours. Do you think it's possible?
Even if dmt become a water soluble salt, it can not be purified in this form?

you add acid to the solution, you get a salt, not free base. you can purify the salt with cold pet ether

also with acetone?
PS. I was thinking about another method for re-x. If I add acid that as you say becomes a water soluble salt, put in water, and basify with NaOH in a ice bath... could dmt precipitate as free base? and separeted by filtration?

 

[pitubo]

I used this tek so many times for purify my crude roto-evaporate caffeine crystal (with warm/hot acetone and pet ether drop by drop) and i used too for ricrystallization of capsaicine and piperine (but i dont remeber if i used the same solvents).

Thanks for the reply. I was really curious when you said your used acetic acid as a polar solvent for freebase alkaloids and then mix than with petroleum ether. It didn't make sense to me.

I think you can use the multisolvent technique together with the freeze precipitation commonly used here. Simply chill the acetone solution and drip in ice cold petroleum ether. You may not get the same yields as you would from dissolving in hot petroleum ether only and freezing that. But that is just a hunch, I have not done a side by side comparison.

PS. I was thinking about another method for re-x. If I add acid that as you say becomes a water soluble salt, put in water, and basify with NaOH in a ice bath... could dmt precipitate as free base? and separeted by filtration?

You should search the forum a bit. People have been trying this and there are some threads about it. AFAICR it did not work really well.

 

[1ce]

I used this tek so many times for purify my crude roto-evaporate caffeine crystal (with warm/hot acetone and pet ether drop by drop) and i used too for ricrystallization of capsaicine and piperine (but i dont remeber if i used the same solvents).

Thanks for the reply. I was really curious when you said your used acetic acid as a polar solvent for freebase alkaloids and then mix than with petroleum ether. It didn't make sense to me.

I think you can use the multisolvent technique together with the freeze precipitation commonly used here. Simply chill the acetone solution and drip in ice cold petroleum ether. You may not get the same yields as you would from dissolving in hot petroleum ether only and freezing that. But that is just a hunch, I have not done a side by side comparison.

PS. I was thinking about another method for re-x. If I add acid that as you say becomes a water soluble salt, put in water, and basify with NaOH in a ice bath... could dmt precipitate as free base? and separeted by filtration?

You should search the forum a bit. People have been trying this and there are some threads about it. AFAICR it did not work really well.

Yeah, I use a multisolvent system / rotovap for these extractions. Hell I even store it under nitrogen when I can't be in attendance.

Use a solvent that's better for extracting, and selectively alternate to a different one to refine your product. Use a slow crystallization as your final purification step.

 

[fabio88ct]

Yeah, I use a multisolvent system / rotovap for these extractions. Hell I even store it under nitrogen when I can't be in attendance.

Use a solvent that's better for extracting, and selectively alternate to a different one to refine your product. Use a slow crystallization as your final purification step.

Hey 1ce,
could you explain in detail your tek? if you had a solution of petroleum ether/dmt freebase, that comes from separating funnel (liq/liq extraction), how do you do?

 

[1ce]

Yeah, I use a multisolvent system / rotovap for these extractions. Hell I even store it under nitrogen when I can't be in attendance.

Use a solvent that's better for extracting, and selectively alternate to a different one to refine your product. Use a slow crystallization as your final purification step.[/quote]

Hey 1ce, 8
could you explain in detail your tek? if you had a solution of petroleum ether/dmt freebase, that comes from separating funnel (liq/liq extraction), how do you do? [/quote]

I do not use diethyl ether. At least not for dmt extraction. I use TCM as a primary solvent, and neptane as a secondary. TCM(chloroform) is easy enough to prepare for even the most novice chemist. It's extremely dirt cheap (I think enough for a 100g extraction costs me about 98 cents).

It is safe enough for any kitchen chemist, and requires no watched/dangerous chemicals. If a mod approves I'll elaborate on it. Chloro extracts like a champ!

Edit: I did the math, it costs me ~68 cents to prepare enough dmk for a 100g extraction.

 

[1ce]

Another thing, IIRC, I remember hearing once that if you have relatively pure DMT freebase, you could dissolve it into diethyl ether and crash it into hexane to form spontaneous rhomboid crystals. I've never tried it (now I feel tempted to). Perhaps another member here could comment on that.