Hot solvent + hot mimosa?

[Smoker root]

Hi I bought my first hot plate stirrer(until now I only had a magnetic stirrer) and want to extract some DMT.

I usually do typical A/B extraction, acid, base, hot solvent sep funnel shake.


But I thought of using the hotplate. Heat the solvent add to mimosa stirr in hot plate, keep at that temp for 15min. Go to sep funnel, let two layers form, shake and sepparate

How will it go? Better yields? Less pure product?

 

[Hailstorm]

With a hotplate stirrer you don't need a separatory funnel, assuming you filter the bark out before you basify the solution.

Add the non-polar solvent to the basic water, create a vortex, wait a bit. Stop the stirrer, wait for the layers to separate and emulsions to settle (happens quickly if the pH is 13+ and the liquid (not surface) temperature is 60-70C). Use a pipette or syringe to collect the solvent layer. Repeat several times and you are done.

The heat will help the yield, reduce the amount of solvent required, but will also decrease the purity.

Safety tip: you do not want any lye splashing out. So avoid any extremes: do not cap the vessel airtight, do not go crazy with the stirring speed, do not heat the solution up to boiling. Leave some headspace in the flask and break up the foam if starts blocking the vapors.

Purity tip 1: The layers do not actually separate fully - there will be tiny droplets of water in your non-polar solvent (and vice versa) - the closer to the separation line, the dirtier the solvent is. It means you will end up picking up some water and lye particles even if you are extra careful. (This is why dryteks produce cleaner DMT than wet teks, by the way - liquids separate from solids much better than they do from other liquids). To minimize that contamination stay as far away from the separation line as you can (especially since you will keep adding more solvent anyway). Transfer the solvent to a tall measuring cylinder first, and wait for any gunk, visible and invisible, to sink to the bottom. The top part of the cylinder should be good enough to transfer out. The cylinder is reused, so you will not lose much overall.

Purity tip 2: I recommend defatting after you filter the bark out. Just follow the same exact procedure a few times; here instead of DMT you will extract plant oils and other non-polar impurities. Since the solution is still acidic, the emulsions will take much longer to resolve.

Purity tip 3: I also recommend a sodium carbonate + water wash before you finally evaporate and/or freeze-precipitate. It can be done in a smaller flask, with manual swirling. It will reduce the yield, so if you have never done it before - skip this step, collect and weigh the final product first, and then redissolve and wash it to see how much you lose and if you are OK with that.

 

[Smoker root]

First of all, thanks for answering!. Hope you are safe.

With a hotplate stirrer you don't need a separatory funnel, assuming you filter the bark out before you basify the solution.

Add the non-polar solvent to the basic water, create a vortex, wait a bit. Stop the stirrer, wait for the layers to separate and emulsions to settle (happens quickly if the pH is 13+ and the liquid (not surface) temperature is 60-70C). Use a pipette or syringe to collect the solvent layer. Repeat several times and you are done.

I think that temperature is too much, I think it is apropiate to kept the mixture of nafta and mimosa at the temp of the nafta(35) just to make it more efficient. I am talking about a setup with a beaker, a thermometer and the plate the extraction is not going to be too efficient without shaking.

Purity tip 2: I recommend defatting after you filter the bark out. Just follow the same exact procedure a few times; here instead of DMT you will extract plant oils and other non-polar impurities. Since the solution is still acidic, the emulsions will take much longer to resolve.

Mimosa hostilis has not got many oils as the confusa. I belive defating is a waste of solvent, since most of the times you end up recrystalizing from heptane in where you get rid of the oils.

Purity tip 3: I also recommend a sodium carbonate + water wash before you finally evaporate and/or freeze-precipitate. It can be done in a smaller flask, with manual swirling. It will reduce the yield, so if you have never done it before - skip this step, collect and weigh the final product first, and then redissolve and wash it to see how much you lose and if you are OK with that.

Wow that is a new one for me. I have been always ectracting in a lab that way (bicab wash or salt wash, water and then dry with magnesium sulphate) However, I never though of using it in DMT extraction. I belive this will help getting rid of the fats right? Thanks.

Btw I have just know have problems when drying as the dmt oxidised. How do you dry it? Would drying under vacuum work?

 

[Hailstorm]

I think that temperature is too much, I think it is apropiate to kept the mixture of nafta and mimosa at the temp of the nafta(35) just to make it more efficient.

A broad range of temperatures is going to work, it is just a matter of how much solvent can absorb all the DMT.

I prefer heptane to naphtha - it is less stinky, less toxic, and it evaporates faster. You can see the solubility curve of DMT in heptane here. As you can see, at room temperature DMT is poorly soluble in heptane, and to avoid wasting too much solvent it is recommended to heat it. DMT seems more soluble in naphtha at lower temperatures, so heat is less important with naphtha.

I belive defating is a waste of solvent, since most of the times you end up recrystalizing from heptane in where you get rid of the oils.

I did not find it easy to get rid of non-polar impurities with recrystallization - their solubility curves seem similar to that of DMT itself.

I belive this will help getting rid of the fats right? Thanks.

No, a carbonate/bicarbonate wash gets rid of lye particles and other polar impurities that make their way into the solvent. It results in better smell and smoother vapor.

How do you dry it? Would drying under vacuum work?

Vacuum drying is the best way, but a usual fan is good enough. DMT degradation takes time, so it is more important to store DMT freebase in a dark, cold container with oxygen absorbers than it is to worry over the few hours of drying. If converted to the fumarate salt DMT is said to be very stable even under normal conditions, and I suspect DMT tartrate is similarly stable as well.

 

[Smoker root]

No, a carbonate/bicarbonate wash gets rid of lye particles and other polar impurities that make their way into the solvent. It results in better smell and smoother vapor.

Great. You wash with bicab, then water, then dry? Or how?

 

[Hailstorm]

There are teks posted on the wiki here.

Basically shake the non-polar DMT solution with a small amount (say, 10% of the total volume) of saturated NaCO3, pipette the bottom layer out, then wash it twice more with distilled water.

 

[Smoker root]

There are teks posted on the wiki here.

Basically shake the non-polar DMT solution with a small amount (say, 10% of the total volume) of saturated NaCO3, pipette the bottom layer out, then wash it twice more with distilled water.

Can you link any? I usually use the same volume

 

[Smoker root]

There are teks posted on the wiki here.

Basically shake the non-polar DMT solution with a small amount (say, 10% of the total volume) of saturated NaCO3, pipette the bottom layer out, then wash it twice more with distilled water.

And besides. Won't having some water in the solvent complicate freze prep?

 

[Hailstorm]

Carbonate wash. Discard all the water and freeze-precipitation will work fine. If you wash after freeze-precipitation and not before, then you can slowly (keep it mostly covered) evaporate it.