02-17-02 03:28
No 270834
I have some problems with crystallizing DMT,i used the route tryptamine+iodomethane in IPA __>quarternarry ammonium iodide and boiled 10 gram of this salt in 40 grams ethanolamine (very cheap and easy to get)
deluted this with 100 ml water and extracted this 3 times with 50 ml ethylacetate and washed the extract 2 times with 50 ml water dryed the ethylacetate with MgSO4 and destilled 110 ml of ethylacetate under reduced pressure untill i got circa 40 ml of ethylacetatesollution,and now i have some problems to crystallize the DMT,can anybody help me out with this problem because i does not want to crystallize,any tips or tricks?
(Hive Addict)
02-17-02 04:54
No 270847
DMT (freebase) is a bitch to crystalize. A/B extractions help.
(Stranger)
02-17-02 06:58
No 270871
usually it is small amts of crap that is contined in the solution that prevents crystalisation, try adding a little charcoal filter off the charcoal, then concentrate the filtrate as much as possible, stick a bit of glass rod in it scratch it around a bit and put it in the freezer. leave for a day or two, if it still hasn't xtalised try slowly warming to room temperature whilst stirring with the rod.
there are more involved ways, stripping all the solvent then vacuum distillation using an oil pump always works.
from memory d distills at 145 at 3mmHg
there are of course millions of other other tricks
(Moderator)
02-17-02 11:06
No 270917
It has a very low mp and doesn't crystallize from raw ethyl acetate solution. Usually it is a waxy solid. Vacuum distillation would be good way to purify.
(UTFSE)
(Stranger)
02-17-02 11:22
No 270926
lillienthal,I do understand that if you have a highvacuumpump and shortpath dest. equipment that it no problem but at this moment i don`t,so I`m looking for a alternative route to get the jobe done.i though to go for the picratesalt and purify it this way and turn it back to the freebase,but which solvents can be used to crystallize DMT freebase from,any sugestions?
(Moderator)
02-17-02 11:40
No 270930
Picrates are a big nono in pharmacology... Maybe tartrates? Or oxalates from THF?
A distillate / plain oily substance will crystallize / solidify over time.
(Hive Bee)
02-17-02 12:06
No 270941
I once made the fumerat, disolve in methanol and ro.vap.
I think the best solvent to rextalice is cyclohexan, disolve and let it stand in the freezer over the night
(Newbee)
04-19-02 20:38
No 299388
Crystalizing Tryptamines can be very tough. If you can't vacuume distill, and you don't have a seed crystal, it can be tougher still. I've heard tales of guys waiting for months or even years for crystalizations to take place. Your post was a while ago, but it is possible, that you still don't have crystals. Here are two possibilities, get rid of solvents, and try to crystalize a little from boiling water. Just heat it up and let it sit for awhile cool. Another possibility is forming a hydrochloride. Careful, indoles don't like strong acids. But, sometimes it is the the way to go. I once synthesised a tryptamine derivative, vacuume distilled it to purify it, and waited patiently for about a month, but to no avail. Completely pissed, I introduced said material to dropwise addition of cold concentrated HCL with stirring. Crystals formed immediatly. I rinsed um off real well, and later released the free base, by heating with sodium bicarbonate in H2O. The base solidified immediatly upon cooling. Primitive, but effective. The tryptamine involved was not DMT. So, don't risk burning up all of your product, its no gimmie. Also, watch that PH. As long as the free amine is gobbling up HCL, the 2 position on the indole ring should be pretty stable. Should the PH become very acidic, bad things might happen.
(Hive Bee)
04-21-02 13:54
No 299864
GOD doesnt know shit about these types of synthesis, but has dreamed of extractions with CONSISTANT white crystals (they acquite the slightest tinge of orange when finsally scraped up with a razor) formed upon evaporation of freebase dmt.
He uses r*s****l brand lighter fluid (naphta)
works every time...
BEND OVER AND PROSTRATE YOURSELVES BEFORE ME!
(Chief Bee)
09-19-02 17:43
No 358308
It does not work as advertised, see Post 126957 (Lilienthal: "Breath of Hoax? / PTC tryptamine alkylation on the test bench", Tryptamine Chemistry)
(Stranger)
10-06-02 11:05
No 365080
The best way to crystallize DMT is to dissolve it in hexanes, then strip off the hexanes in vacuo. Magically, this normally difficult compound crystallizes out very nicely as a waxy off-white solid.
(Hive Bee)
02-26-03 02:53
No 411891
Just verifying lil's assertion about tartrates. Very effective made acacia extract into crystals (this is *NEW* pictures coming soon goddammit!)
And freebases crystallising. man, such a pain. Yes, give it time. the bases hold onto the solvents very hard because of such a little difference in bp/mp. Personally, I'm never ever again going to even *try* smoking dmt freebase. Didn't help much I had rough extracts that still probably had some hydroxides in them, but after 4 times gettin well trippin on IV dmt (mostly tartrate but first tiem with acetate) - no way. My lungs don't like burny alkali stuff. No matter how pure (goddammit!). IV kicks ass.
I know naaaathing.