completely dry out basified solution and wash powder with hexane

[JJ Spigglesworth]

Hello all

As this is my first post I'll start off with a massive thanks for everyone who has contributed to this forum - It's been an amazing resource for my first steps with DMT.

Here's where I'm at. I've got a reasonable yield from an acid/base extraction using vinegar for the acid soak and NaOH for the basification. The 4 naphtha pulls have yielded around 0.5g from 100g of mimosa after freeze precipitation.

now for the Q:
do you think it is a good idea to evaporate the water from the lye solution to leave a powder containing DMT, lye and all other components that were dissolved in the basified solution? It should be possible then to wash the resulting powder with hexane to extract the last bit of DMT.

Am I missing something? the pH would increase drastically until the lye began to precipitate, would this break down the DMT? would the mild heating required to evaporate the water vaporise the DMT?

thanks in advance for any advice you can offer

JJ

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The above discussion is purely theoretical and written in the first person for the sake of convenience.

 

[endlessness]

Sounds messy and energy-inneficient imo... Other options:

1- Do another couple of pulls, leaving each for a day or two, with a lot of mixing whenever you pass by and remember, finishing with warming up the whole thing in a waterbath and doing one last mix and then separating the pull. If they yield something, keep pulling

2- Using another solvent like limonene, xylene, toluene, which pull more alkaloids, then salt them out and purify if desired.

Also, since you didnt say the amount of mimosa and of your pulls, I dont know if ratios were appropriate. If you used too much naphtha, maybe it wasnt saturated enough for freeze precipitation, and you needed to pre-evap. Hopefully u still have the naphtha and can evaporate it down to small amount, like till a quarter is left, and freeze again to see if more comes out, or just reuse that naphtha.

 

[benzyme]

the pH would increase drastically

how do you figure? NaOH has a solubility constant, so while it would precipitate as you evaporate water, the pH would not increase.
It would not make any sense at all to evaporate your aqueous phase, as phase transfer of your product occurs across the biphase interface. this is a liquid-liquid extraction. you won't get the same effect from a precipitated solid phase combined with a nonpolar.

 

[JJ Spigglesworth]

Thanks for the quick response!

I started with 100g mimosa, and each pull was around 100ml of naphtha (colemans fuel) left for 24h each. I evaporated the solution until it became cloudy, then placed in the freezer (around -25C) for 24h to crystallize. I still have the naphtha, in fact it's back in the jar for another pull anyway.
I've been avoiding heating so far, but I'll try that on this final pull after a couple of days of regular mixing.

I'll also try to get my hands on some other solvent, but it's not easy to find clean-evapping ones in the UK!

My question was more theoretical really. once I've got all I can out of solution with solvent extrations I can see no reason not to evaporate the NaOH solution and see if there's any product left unless doing so would destroy the DMT. Energy efficiency is not really an issue since the heating is on anyway!

 

[JJ Spigglesworth]

benzyme - my NaOH solution is currently not saturated, so the pH will increase up to the saturation point.

I guess the real q is: Is DMT stable in a solution saturated with NaOH?

as DMT is not particularly soluble in H2O it shouldn't it also preciptiate, ready to be re-dissolved in a non polar slovent?

 

[benzyme]

destroying the DMT isn't the issue, it's application of the technique.
again, there's no good reason to evaporate the aqueous basic phase.

 

[benzyme]

benzyme - my NaOH solution is currently not saturated, so the pH will increase up to the saturation point.

have you tested this theory?

DMT won't be affected too much, it's a stable compound, that may oxidize a bit above pH 13.6;
but even that product is active.


test your theory, its the only way to find out for sure. I venture it's not an efficient approach at all, especially using a solvent like naphtha.

 

[JJ Spigglesworth]

Of course you are correct, NaOH concentration will increase but not necessarily pH

Thanks for your advice. I probably won't bother with the evaporation unless i'm bored and fancy experimenting before I dispose of it. If I do I will post the results here which will no doubt confirm what you have suggested.

It's good to know that DMT is stable at high pH, should I ever need to reduce the volume of my basic phase in the future.

Thanks again!

JJ