Re-crystilization Related Question

[josboaz]

Hello,

I'm reading the re-crx step of this DMT extraction T.E.K. it's talking about heating the solvent to dissolve the freebase DMT, when that is done the impurities would drop down at the bottom.

But I was wondering what would happen if I dissolve the DMT into acid and then place it in a cold solvent, would that also work? or can I dissolve the FB DMT into acid and then base it and then add the base liquid to the solvent, will that also cause the separation of impurities? because I'm not too keen on heating flammable solvents.

 

[Jan e Kharabat]

Dissolving freebase DMT in aqueous acid will convert the the freebase into a salt. For example, if you dissolve DMT freebase into vinegar/acetic acid, the freebase will be converted to DMT acetate, which will readily dissolve in water. To convert it back into freebase, you can add a base to the solution. After that there are multiple ways to get the freebase back, one is to put the solution in a fridge and wait for the water insoluble freebase to crash out. The other, which is my preferred method, is to add the NPS, shake, and pull. Depending on you starting amount, you will have to do 2-3 pulls with minimum amount of solvent. You can then put the solvent in the freezer and freeze precipitate the freebase. This is called a mini A/B. In my experience, this is a much more efficient way of purification than a simple re-x.

 

[josboaz]

Dissolve DMT freebase into vinegar/acetic acid, the freebase will be converted to DMT acetate, which will readily dissolve in water.

Can I at this stage, filter this liquid through a funnel with a cotton ball to remove the impurities, and then base it and place it in the freezer?

I mean how do I remove the impurities at the acid part if I simply base it again without filtering it? The junk just stays in the solution, and when the crystals crash out they will drop to the bottom, exactly where the impurities would be laying. So I would assume I need to filter it at some point. Just like the filtering at the Manske stage of Harmala extraction.

 

[fink]

On the heating solvent thing. Put it in a small glass vessel then put that vessel in a bigger bowl of hot water. A few minutes and the NPS will be plenty warm enough.

 

[Jan e Kharabat]

If you see any impurities, like a fatty layer swimming at the top of the aqueous solution or any particles settled at the bottom, then filter and pour some water through the funnel to recover anything trapped in the filter. If you don't see any impurities, then filtering won't do anything. When you'll base, a layer of fat may appear but when you'll pull this time, the solvent would dissolve a much smaller amount of those impurities and a much more significant amount of DMT. In mini A/B, the pulls are much easier, no need for prolonged shaking or heat bath, and you can just do 3x 30-50ml pulls, you'll get all the DMT and most of the impurities will be left behind.

One thing you should keep in mind though, is that sometimes when you add the base and shake, clumps of brown DMT precipitate almost instantly. Those are not impurities, just DMT! So, generally speaking, after basing, don't worry about any visible impurities, just add the solvent, shake and pull.

 

[josboaz]

On the heating solvent thing. Put it in a small glass vessel then put that vessel in a bigger bowl of hot water. A few minutes and the NPS will be plenty warm enough.

Yes that I can do, but the T.E.K. stated I need to place the solvent jar in a pan with water and then heat the water until the solvent starts to boil.

 

[josboaz]

In mini A/B, the pulls are much easier, no need for prolonged shaking or heat bath, and you can just do 3x 30-50ml pulls, you'll get all the DMT and most of the impurities will be left behind.

Alright so if I understand it correctly, after the first freebase is created. Just place the crystals in acid, then base it, then place it in the freezer, scrape the newly created freebase, and do this step 2 more times. Without the need for filtering it through the funnel with cotton?

 

[fink]

On the heating solvent thing. Put it in a small glass vessel then put that vessel in a bigger bowl of hot water. A few minutes and the NPS will be plenty warm enough.

Yes that I can do, but the T.E.K. stated I need to place the solvent jar in a pan with water and then heat the water until the solvent starts to boil.

Well maybe. But you really dont have to do it that way for a simple re-x.

 

[josboaz]

A few minutes and the NPS will be plenty warm enough.

What does NPS mean, does it mean Naphtha Solvent?

 

[benzyme]

A few minutes and the NPS will be plenty warm enough.

What does NPS mean, does it mean Naphtha Solvent?

Nonpolar solvent

 

[Jan e Kharabat]

Take a small bottle that can be tightly closed, with a lid which won't be affected by the NPS, add the impure freebase to it, add some aqueous acid and shake until it dissolves, basify it, add small amount of NPS, shake, let the layers separate, shake twice more, once the layers separate the third time, pull out the NPS, do 2 more pulls or until the milkiness of the solution is gone, put the NPS of all the pulls together and put it in the freezer. The NPS is what goes into the freezer, not the basified solution, unless you want to precipitate straight out of the aqueous solution (which... Is not my preferred method for various reasons).

 

[josboaz]

Take a small bottle that can be tightly closed, with a lid which won't be affected by the NPS, add the impure freebase to it, add some aqueous acid and shake until it dissolves, basify it, add small amount of NPS, shake, let the layers separate, shake twice more, once the layers separate the third time, pull out the NPS, do 2 more pulls or until the milkiness of the solution is gone, put the NPS of all the pulls together and put it in the freezer. The NPS is what goes into the freezer, not the basified solution, unless you want to precipitate straight out of the aqueous solution (which... Is not my preferred method for various reasons).

Ok thanks, I will do so, thank you for the clear instructions