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Peltier recrystallization probe

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foaf

foaf

Rising Star
So I had an old extraction that I left that was maybe 90% spent and was gonna throw away, but with mhrb not easy anymore, I decided to work it some more. It was 5 gallons of lye/bark that had sat in the sun to fester for a year. I wanted to experiment with the zinc dust dmt oxide reduction on it, and the zinc dust/formaldehde nmt -> nndmt conversion since who knows what happens in a year in the sun at ph 11. And these teks will possible be helpful with Acacia which is thought to have a lot of NMT and which I am working on a big batch of right now too. The yellow/orange Oil that I got out of it measured 20 grams. None would crystalize. Smelled of DMT. I realize that ther is no reason to know or believe NMT was in here, but ther was reason to believe there was DMT oxide. And I wanted to at least do dry runs of the reactions. Nothing to lose.
 

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I took half and boiled it in vinegar with an equal weight of zinc dust. The premise being that you can convert DMT N Oxide into NN-DMT. The reaction proceeded quickly in that the orange appearance cleared in just a few minutes. I ran it at boiling for 20 minutes with stirring and then extracted after basifying with KOH using DCM. I got a clear oil that smelled of dmt and wouldnt crystalize. I know people react it longer, but I have yet to see a picture validated success anyway so who knows.

The other half I did the same thing but added 3x stiochiometric formaldehyde to react with any NMT that might be present. Same thing happened.

The milky picture is what both basified aqueous phases looked like after the zinc or zinc/formaldehyde reaction extracting with DCM and evapping.
 

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So I gathered the 20 or so grams of now clear oil like uncrystallizable goop from my playing around and used it to test my new recrystallizer toy. I plan to use it as part of my Acacia extracition that Im working on now.

So a CPU heat sink from the attic. A stainless steel bolt welded to a 3/16 steel plate. A 90 watt 12v peltier chip from ebay, cheap. Heat transfer paste. cotton insulation and teflon tape over it. Put in a jar and play around with it.
 

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nice application of peltier :thumb_up:

Do you stirr liquid in the jar?
What's the temperature of water around the jar?
 
As there is little proof of the reduction being done there isn't much to be said there. However, you're recrystalization probe is a wonderful little device! What kind of temperatures can be maintained using it? Keep it up!
 
As there is little proof of the reduction being done there isn't much to be said there
Click to expand...
.

sure. I have no idea exactly what I started with or what if any useful reactions took place. Just wanted to define what the starting material was for the recrystallization.

As far as temperature. I warmed the heptane and clearish goop up, stirred, let it get to about room temperature, then put the probe in and let it sit for 24 hours in the pictures, now 48 and more crystals adding on. I took the probe out today, heated and stirred the solution, let it cool to room temperature and settle, and put the probe back in.

The probe stays about 45 degrees when the room is at 70.

I am saving samples of each step and as I play around with tlc and work out a solvent system that I am happy with, Ill see if I can clarify anything.
 

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this is one of the nicest posts iv seen in a while - good job

i did much the same using a U shaped peice of glass attached to a water pump cycling cold water through it - the outcome was the same. for the reduction in the past, zink/hcl was used
 
Phlux- said:
this is one of the nicest posts iv seen in a while - good job
Click to expand...

i agree

thanks for posting this, foaf

edit : one question, can someone post a link where it explains what is the science behind this crystallization technique ? or the name of the method used in literature ?
 
A good solvent system for amines is usually ethyl acetate 10 : 1 methanol. or 20 : 1. Both of these solvents are found locally in the US without issue. For tricky ones a little bit of ammonia can be added. Love to see some TLC plates :)
 
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