D Limonene & backsalting

[urtica]

Hey folks-

I don't know if this is the best place for this question, but has anyone had trouble backsalting when using D limonene as the NPS?

I have been doing some work with various Trichocereus clones to determine which of them have usable/extractable amounts of mescaline & other phenethylamines.

I have been using the a/b tek from the wiki, kash's. This tek calls for xylene as the NPS, which I cannot stand the smell of so I switched to D limonene.

The last extraction I did had an obvious precipitation when I basified the acidic tea of the cactus, looked like alkaloid crashing out.

I extracted this tea with D limonene 4x and watched the precipitate leave the tea & the limonene cloud.

I backsalted 2x with an HCl solution which was certainly acidic enough, combined & evapped, only a bit of goo.

I distilled off the d limonene to leave a clear/yellow thick oil which tastes bitter. Could this be mescaline freebase that did not go into the aqueous phase during backsalting? If I dissolved this in say 95% EtOH & acidified with HCl would that convert it back to the HCl form?

Any help appreciated.

~u

 

[Mindlusion]

Hey folks-

I don't know if this is the best place for this question, but has anyone had trouble backsalting when using D limonene as the NPS?

I have been doing some work with various Trichocereus clones to determine which of them have usable/extractable amounts of mescaline & other phenethylamines.

I have been using the a/b tek from the wiki, kash's. This tek calls for xylene as the NPS, which I cannot stand the smell of so I switched to D limonene.

The last extraction I did had an obvious precipitation when I basified the acidic tea of the cactus, looked like alkaloid crashing out.

I extracted this tea with D limonene 4x and watched the precipitate leave the tea & the limonene cloud.

I backsalted 2x with an HCl solution which was certainly acidic enough, combined & evapped, only a bit of goo.

I distilled off the d limonene to leave a clear/yellow thick oil which tastes bitter. Could this be mescaline freebase that did not go into the aqueous phase during backsalting? If I dissolved this in say 95% EtOH & acidified with HCl would that convert it back to the HCl form?

Any help appreciated.

~u

Tasting bitter is a good sign, but no one can tell you exactly what it might be, it could be nothing.

you should go ahead and give it a try, extracting that into acidic phase, it can't hurt.

You could try precipitating from ethanol, but id be concerned about not getting precipitate.

I would digest it into acidic water, some HCl water, lots of stirring and a bit of heat, (microwave is great).

Then add a bit of nonpolar solvent hexanes preferably or a bit a limo, to wash it and pull out the gunk, then evap the water layer

Basically extract it again to see if you missed anything, you could just have a poor yield, or the goo is denser than you think

 

[urtica]

Ok, thanks!

Have you ever backsalted from d limo? Did it work fine? I feel like I have heard a bit about it not being the most useful nps for some reason, is that one of them?

Thanks again!

 

[urtica]

Hmm, maybe I should wash the acidic water after backsalting in general, I always thought that the backsalt was basically defatting, but I have gotten some really gooey extracts after the first couple...

 

[Mindlusion]

Hmm, maybe I should wash the acidic water after backsalting in general, I always thought that the backsalt was basically defatting, but I have gotten some really gooey extracts after the first couple...

Yes it is always a good idea to wash the acidic extract with NP, that is the defat.

I don't use d-limo, id use toluene , xylene, or methylene chloride, the latter is the best to use for washing acidic phase or extraction if you use a sep funnel since it sinks to the bottom.
d-limo has a few disadvantages, it is reactive enough to be oxidized in open air, compared to aromatic solvents which are very inert, its not very volatile, it's prone to emulsions, can leave traces in end product, and it stinks too much like oranges for my taste. I can't speak too much about its usage though since I've never actually bothered to use it.

 

[downwardsfromzero]

Limonene, while smelling better than xylene, can indeed be something of a nuisance to use for the reasons outlined above. Mescaline can be a bit tricky as the freebase is appreciably soluble in water.