LSA extraction

[lycaeumblik]

Hello,

1) Extracted 500 HBWR in anhydrous MeOH for 7 days.
2) Evaporated filtrate under vacuum, resulting in orange oily substance and a bit of seed material
3) Redissolved in ddH20, easily dissolved with some shaking / agitation. Extract turned white-ish. When fully dissolved solution looked akin to a colloid of absinth and water with slight green hint.
4) Proceeded to filter this, and resulting solution was relatively clear but still retained green tint.
5) Solution was basified with 1ml of 1N NaOH
6) Solute was mixed with half the volume of chloroform
7) Organic layer was dried under vacuum to yield white crystals.

Now this is where SWIM had some what of a brain fart

8) tried to redissolve in ddH20 and absolute EtOH (2:1)
9) extract was almost completely insoluble.
10) acidified to try to increase solubility with 1N HCL, with no observable change in solubility
11) basified with 5N NaOH, and had a slight increase in solubility with the water layer developing a slight green tinge.
12) added xylene to extract freebase (1:2), and remaining extract easily dissolved in organic layer.

So at this point, SWIM thinks the actives are still in the organic phase. Any suggestions on next steps? I was going to isolate the organic phase, treat with dilute HCL, and evaporate off solvent. Im assuming that the result of which will be much more soluble in ddH20 and EtOH. What do you think?

 

[LysergicMissioner]

that doesn't seem like lsa.

try to dissolve it in ethanol again, and shine a blacklight on it. it should glow something like this

where did @frobot go wrong in his step by step?

And what vaccuum pump is acceptable for extractions? would a single stage pump with 3 gallon collection chamber do the trick?

 

[Vreality]

that doesn't seem like lsa.

try to dissolve it in ethanol again, and shine a blacklight on it. it should glow something like this

where did @frobot go wrong in his step by step?

And what vaccuum pump is acceptable for extractions? would a single stage pump with 3 gallon collection chamber do the trick?

it depends what youre trying to dry out of your solvent is how strong of a pressure / combination of applications to achieve your desired result. checking boiling points of your solvents in question against a vacuum chart for the given solvent will give you some of the insight you are looking for, there are charts with most of the popular solvents one would be evapping on it.

I dropped an example image below if it works..

 

[benzyme]

I'll elaborate for the casual kitchen chemists, because that graphic is esoteric.
to evap low boiling solvents like pet ether, VM&P, hexanes, and heptane, an aspirator or diaphragm pump works.
for higher boiling solvents like toluene, xylene, limonene, and other aromatics, bees have traditionally used Yellow Jacket vacuums... rotary vane.

the former pumps typically have hose barbs, the latter use KF/NW-convention fittings.

 

[benzyme]

I have one of these, I run it with the rotavap.
and that's a pretty good price for one. that lil pump makes xylene boil at room temp.
it has KF-16 flanges.

 

[pastanostra]

I have rread that LSA can photo sensitive and light can alterate the molecule, is it true?
Should we consider doing extraction of LSA with no light ?

 

[benzyme]

LSA is somewhat stable, although it does readily isomerize. I've seen solutions turn amber after a day or two, but that may have been exposure to air and/or light.

would be interesting to do an experiment, where one aliquot is purged with an inert gas and wrapped in foil (or stored in actinic (amber) glass) , and another aliquot is exposed to ambient light and air.

 

[Vreality]

LSA is somewhat stable, although it does readily isomerize. I've seen solutions turn amber after a day or two, but that may have been exposure to air and/or light.

would be interesting to do an experiment, where one aliquot is purged with an inert gas and wrapped in foil (or stored in actinic (amber) glass) , and another aliquot is exposed to ambient light and air.

i'd be happy to do the experiment with my extraction results in success.. I only wish to achieve the results desired with some level of efficiency , I am okay with donating my time and materials for results we can all enjoy as new as I maybe at some aspects of things, time is something I have very much of to dedicate to this end of things.

 

[benzyme]

I'd be willing to do a couple test runs to the cause, on the house, out of scientific curiosity. if anyone could donate a small amount of cyclodextrin (or I may just order some), it would be very helpful. Cyclodextrin acts as a complexation reagent, to aid in separation of isomers. HPLC would show if any degradation/isomerization occurred.

 

[KloudQ7]

I got a free 20 gram sample of captisol/B-cyclodextrin from a pharmaceutical company, not sure if I can say where though. I've used it to make some dabs water soluble and to complex some salvinorin A.

 

[LysergicMissioner]

i'd like to venture with you all in the aid of furthuring our community but i am not confident in my work enough to present some ground breaking results. but good luck and thank yall!PLEASE POST RESULTS!
@Byzeme and @Vreality

 

[LysergicMissioner]

(delete)
mistaken post