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DET synth. problems
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jory

Joined: 22 Apr 2005
Posts: 20
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DET synth. problems

 Fri Apr 22, 2005 12:54 am		 Reply with quote
hello,

SWIM was make DET from TIHKAL (via indole). After LAH reduction he get nice violet fluorescent solution DET in THF (anybody have simmilar experiences? tryptamines fluorescent?). Well, next SWIM generating HCl (H2SO4 + CaCl2) and bubbling solution DET in diethyl eter (after evaporating THF). Some red tar and off-white crystals create. SWIM dissolve it in methanol, solution makes red.
And what next? SWIM wants to get pure crystals, but crystals dont want crystalize. Anybody can help SWIM ? ANYbody have simmilar experiences?
thanks

j.
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Vitus
Psychoscientist
Joined: 19 Apr 2005
Posts: 72
Location: Dunwich
2608.18 Points
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 Fri Apr 22, 2005 1:57 am		 Reply with quote
As you have a violet solution, this looks like there are impurities present ( it is not the colour of the tryptamine). I think that is why your gassing failed. I have seen this happen when attempting to gas coloured solutions of freebase of other amines.

I would suggest that you evap the methanol, basify the mess and extract with ether.
Dry and evaporate the ether, dilute the dark freebase oil with a little IPA, and titrate with conc. HCl until neutral to slightly acidic. Then flood with dry ether, this way you should be able to get decent crystals of the HCl salt.

Flooding w ether might not even be necessary as TiHKaL indicates that DET.HCl crystallizes spontaneously from IPA.
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jory

Joined: 22 Apr 2005
Posts: 20
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View Single Post3918

 Fri Apr 22, 2005 2:05 am		 Reply with quote
Vitus wrote:
As you have a violet solution, this looks like there are impurities present ( it is not the colour of the tryptamine). I think that is why your gassing failed. I have seen this happen when attempting to gas coloured solutions of freebase of other amines.

I would suggest that you evap the methanol, basify the mess and extract with ether.
Dry and evaporate the ether, dilute the dark freebase oil with a little IPA, and titrate with conc. HCl until neutral to slightly acidic. Then flood with dry ether, this way you should be able to get decent crystals of the HCl salt.

Flooding w ether might not even be necessary as TiHKaL indicates that DET.HCl crystallizes spontaneously from IPA.


thanks. SWIM will try this procedure (he was thinking about it).
violet was only as fluorescent. solution was clear.

when SWIM made mescalin by AlHg reduction of 3,4,5-betanitrostyrene he get very red solution after add some drops of conc. h2so4.

why red ?? swim isnt communist ! Wink

best reg
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Vitus
Psychoscientist
Joined: 19 Apr 2005
Posts: 72
Location: Dunwich
2608.18 Points
View Single Post3921

 Fri Apr 22, 2005 2:18 am		 Reply with quote
Quote:
why red ?? swim isnt communist !



Sounds like "they" have been paying you a visit...

get in contact with http://www.jbs.org/ ASAP! Wink
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