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Recrystallization via Water/Acetone Options
 
gibran2
#1 Posted : 9/2/2010 2:56:31 PM

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I’ve been thinking about alternatives to recrystallization and purification of DMT using NP solvents – the thread here is my first idea. Another idea is the use of a binary solvent. The ideal binary solvent for crystallization is one where both components are fully miscible, the solute is very soluble in one of the solvents and practically insoluble in the other. Acetone + water seems to be a perfect choice.

---- Dissolve DMT in a minimal amount of warm acetone.
---- Add warm water dropwise just until precipitation is observed.
---- Allow solution to slowly cool.

DMT should crystallize. Has anyone ever tried this? Will it work?
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dg
#2 Posted : 9/2/2010 7:07:42 PM
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fyi, those are both polar solovents

not sure if it'll work, also not sure why that'd be better than crashing out with heptane for example

do the work and post results
 
gibran2
#3 Posted : 9/2/2010 7:40:41 PM

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dg wrote:
fyi, those are both polar solovents

not sure if it'll work, also not sure why that'd be better than crashing out with heptane for example

do the work and post results

"I’ve been thinking about alternatives to recrystallization and purification of DMT using NP solvents"

As I said in the first post, I'm looking for alternatives to using non-polar solvents, so of course I would be looking for polar solvents to do the job.
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MelCat
#4 Posted : 8/28/2011 9:26:44 AM

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Did you ever give this a shot?
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Phlux-
#5 Posted : 8/28/2011 10:01:43 AM

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reversed acetone bombing - spice into acetone - add water - out falls cleaner spice.
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MelCat
#6 Posted : 8/28/2011 10:51:40 AM

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Hmmm... I've got some jungle goop that won't harden... I've pulled it with naptha a couple of times to get any nn- out so I might give this a shot on it to see what happens.

Anyone else care to try this out? I'm interested to hear the results...
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fathomlessness
#7 Posted : 1/11/2020 4:41:52 AM

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9 years on, Benzyme with the results:

https://www.dmt-nexus.me...px?g=posts&m=1033964
 
Jees
#8 Posted : 1/11/2020 4:44:22 PM

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fathomlessness wrote:
9 years on, Benzyme with the results:

https://www.dmt-nexus.me...x?g=posts&m=1033964

We should keep an eye on the typical distinctions between the methods, it makes the two different teks.

1) In gibran2's approach the 2 (water and acetone) will purposely stay in a mixed phase:
gibran2 wrote:
...The ideal binary solvent for crystallization is one where both components are fully miscible...

2) In Benzyme's approach the two will purposely separate (due elevated pH of the water, the water and acetone become separated).



 
benzyme
#9 Posted : 1/11/2020 5:46:48 PM

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because acetone has a single proton acceptor, and no donor, it is miscible with water at low to neutral pH, but immiscible at high pH. this is why it can act as an extraction solvent, and a recrystallization solvent for salts.
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fathomlessness
#10 Posted : 1/12/2020 12:03:41 AM

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Jees wrote:
fathomlessness wrote:
9 years on, Benzyme with the results:

https://www.dmt-nexus.me...x?g=posts&m=1033964

We should keep an eye on the typical distinctions between the methods, it makes the two different teks.

1) In gibran2's approach the 2 (water and acetone) will purposely stay in a mixed phase:
gibran2 wrote:
...The ideal binary solvent for crystallization is one where both components are fully miscible...

2) In Benzyme's approach the two will purposely separate (due elevated pH of the water, the water and acetone become separated).


Thanks for clearing that up Jees, I was still unsure if I had understood it all correctly.

is there any trial data to suggest gibran2's tek works as effectively as Benzymes? An uneducated guess would make me think that not all the DMT would crash out of just warm water and acetone.
 
 
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