Removing excess HCl from cacti alkaloids

[JCRG]

When salting cacti alkaloids from toluene, it was thought that 0.1 mM (millimolar) HCl was being used.
Turns out it was actually 0.1 M.

Heat evaporation was attempted, but the end result seems to remain as acid as xenomorph's blood.
Although the crystals seem quite dry, a good whiff will make the alveoli cry (asthma?).

Could re-x help with such an issue?
Or should a second A/B be tried instead?

Thanks and kindest regards.

 

[Prima Materia]

Another basification with NaOH would neutralize the HCl to make NaCl. Seems a logical step to make. Or you could try to wash your alkaloids with solvents. I would have to check which ones are used for that. The info is to be found here on the nexus though.

 

[brokedownpalace10]

In a related question, what would be the easiest way to neutralize the highly basic soup left over from a STB. I have used vinegar, it took a lot (a lot) of vinegar and used that stuff orally once with Harmalas. There's leftover stuff in there.

 

[Prima Materia]

In a related question, what would be the easiest way to neutralize the highly basic soup left over from a STB. I have used vinegar, it took a lot (a lot) of vinegar and used that stuff orally once with Harmalas. There's leftover stuff in there.

You could saturate your basic solution with salt (NaCl) and then extract with IPA. When the basic solution is saturated it should not mix with anhydrous IPA. After the alkaloids are in IPA you can react this in FASI style method to precipitate DMT fumarate out of the solution. DMT fumarate should work mighty fine for oral journeys. Do check all the info by yourself also, there should be plenty of info on the forums.

EDIT: I believe you could do the same with benzoic acid, if access to fumaric acid is an issue. Benzoic acid san very easily be prepared from sodium benzoate which should be readily available as a food preservative. Dissolve benzoic acid in IPA and add that to IPA rich in alkaloids to precipitate DMT benzoate. For oral consumption fumarate salt is most likely prefered.

 

[doubledog]

I would try to wash the crystals with cold acetone.
In general, for salting out the alkaloids from toluene, some liquid pH indicator is of great help.

 

[JCRG]

Another basification with NaOH would neutralize the HCl to make NaCl. Seems a logical step to make. Or you could try to wash your alkaloids with solvents. I would have to check which ones are used for that. The info is to be found here on the nexus though.

Wouldn't sodium chloride in the end result open a whole 'nother can of worms?

I would try to wash the crystals with cold acetone.
In general, for salting out the alkaloids from toluene, some liquid pH indicator is of great help.

A calibrated pH meter was actually used, but its shape prevents it from measuring tiny volumes in confined spaces, like the bottom of a separation funnel.
When there was enough polar phase in the receiving bottom flask, it was already too late (pH measured as 1.98).

 

[JCRG]

In the end H2O was added and boiled off in multiple instances, until no acidic odour was perceived.
HCl remnants seem to be at minimum now!

Let this be a lesson to properly triple check the labeling of solutions, and perhaps confirm with actual measurement.

 

[Prima Materia]

@JCRG after basification with NaOH it would have to be extracted again with toluene and salted out again carefully.