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Clean up the spice precip. from acetone with water Options
 
kemist
#1 Posted : 12/5/2010 9:33:50 AM

John


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Location: Highland
So ILPT done some extraction of a bit dirty mimosa (probably not hostilis, nevertheless cointainig dmt and jungle as previous extraction showed)

He done citric acid cooks , combine and let it decant for few days to seperate the sticky sludge, then filtered boiled down to 1/10 of original volume ,filtered again then added NaOH solution and pulled 4 times with limonene

He salted limo with hydrochloric acid , separated and evaporated the the water layer with aid of fan and hot plate to get reddish oil.


At this point he kept busy for good 6 weeks, so he left it uncovered in little glass beaker at room temp for good 6 weeks So usin heat, a bit old bark stored at room temp. and slowly extracting procedure might well turned most of the DMT into the N- oxide Sad
After 6 weeks he rinsed it once with acetone and kept the acetone only to evaporated it now to gain product numbe I.
The rinsed oily stuff was decanted of all acetone and processed into product II.

I. It has strong smell of limonene but when he heated up he could smell tryptamine reasonably strong.
So what would be solubility of DMT.HCl in acetone?
Presuming there is some dmt.hcl in orangey oily evaporate he added some distilled water and almost everything dissolved. there seem to be about 200 mg of this stuff
He thinking about filtering this solution well then basify to high pH 12 or more and try to pull with hot heptane.
Is it a good idea ?
There is fair contamination with leftover of limonene and oxidized limonene in this part !

II. So some off the acetone stayed in the oily hydrochloride mixture and ILPT didn`t think it would cause any problems, so he just added a bit of dry Ca(OH)2 and mixed well till he get almost dry dough like consistency.
He was afraid that a proper freebasing might not taken the place so he moistened it a bit with water to get clay sticky consistency. Then he added dry Na2CO3 to get back to dry dough like consistenci.
He afterwards crumbled the dough and air dried it on radiator.
After drying he passed it trough the mesh to get finely granulated powder of orangey colour. he rinsed it well with dry acetone until it got white in colour.]
He collected acetone and filtered it prior to the evaporation.
it evaporate into orangey reddish substance which was very sticky and oily but upon smearin it over surface of pyrex dish and drying using warm hotplate and fan it solidified into slightly sticky waxy orange-red substance weighting about 800mg
How to clean up this stuff ?

He did an heptane boil on this stuff and freeze precip to only yield slightly over 100 mgs of dmt yet contaminated with yellow oil
Now ILPT thinking off dissolving this freebased stuff in minimum ammount of acetone and add much more of distilled water to precip some dmt. Is this a good idea ?

Bare in mind that ILPT has only few solvents on hand which is 99,95 % acetone and IPA the little bit of pure heptane and limonene(which he all need for cacti extraction).

he know a/b cleaning would help a lot but he hasn`t got suitable solvents like dash of ether, dcm or toluene

any inputs apreciated. again all chemicals ilpt has at the moment are solvents mentioned above plus citric acid, gar, HCl, NaOH, NaHCO3, Na2CO3 and Ca(OH)2. so he can`t even think about zinc reduction

ILPT can`t find much details on solubility of DMT. HCl and DMT N-Oxide. HCl in various solvents. All he know is they both are soluble in water whic is pretty much obvious.







As a kemist I never met ILPT in physical form and never talk to him. He share his wisdom, trough my mind, telepathicly only. Please don`t prosecute me, for his possible illegal activities. He is bonkers about chemistry and doesn`t even exist in this primitive reality !!!
 

Good quality Syrian rue (Peganum harmala) for an incredible price!
 
benzyme
#2 Posted : 12/5/2010 3:45:42 PM

analytical chemist

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basify to pH of ~ 12
extract with a nonpolar
wash the nonpolar phase with 5% sodium bicarb solution (w/v)
freeze precip
"Nothing is true, everything is permitted." ~ hassan i sabbah
"Experiments are the only means of attaining knowledge at our disposal. The rest is poetry, imagination." -Max Planck
 
 
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