Ethanol freeze precipitated crystals

[modern]

so after a chloroform extraction I ended up using a little excess sulfuric acid which lead to color impurities and pulling other alkaloids. I washed with sieve dried ethanol 2ml at a time and then froze the solution overnight. This lead to a dark precipitate that once reaching room temperature it melted and only some white crystals which I suspect is mescaline sulfate on the bottom. I decided to combine with the 'washed' crystals and added hot ethanol to recrystallize and will freeze again then attempt to separate after. Visually not a small amount of material.

first 3 photos are the first extraction washed with isopropanol which I later recrystallized everything qince I used excess later. Only based on visual volume and appearance the freeze precipitate is insoluble in isopropanol.
photos 4-5 is recrystallized with everything and washed with minimal ethanol in 2ml batches. Not as much color removed compared to original washes.
photo 6-7 is the collected ethanol washes which precipitated after hours in the freezer near absolute ethanol so not ice.
Final photo is the collected crystals from 4-5 quite dirty still.

I'll likely do a mini a/b on this material rather than repeated crystallization. The freeze precipitated crystals were most interesting sofar.

Personally I liked chloroform as the non-polar solvent but had a terrible emulsion due to shaking even after defatting with hexane. I did methanol extract folloqed by acid to remove tar/fats then lye freebase chcl3 pulls and sulfuric acid pull. Original papers would evaporate solvent to dryness which I may attempt next time.

 

[modern]

from 2.1g total crude to around 700mg of pretty thick sulfate crystals. Around .66% yield this is the yield I normally get after excessive cleaning of HCL. The washes have been saved.

I qashed in 2ml batches of Iso99 to keep losses until no color removed. dry ethanol didn't remove any either... did HOT water slow crystallization for the pretty crystals. There qas a small amount of brown water under the crystals and was collected in picture 6. washed once more with dry alcohol and now doing a final water crystallization.

The swirls was interesting pattern from the alcohol washed glass of the crystals. usually get some mini needles not swirls.

 

[DetritusTheEgo]

I need to reread the posts to follow along on your process but the long crystal photos with a twinge of brown are beautiful ( 1331, 1330, 1329, 1323 ). While it must have sucked to eventually break them apart and collect I'm guessing it was oddly satisfying at the same time.

 

[modern]

I actually recrystallized once more in maybe 50/50 isopropanol water solution for these shiney crystals.

I froze all the decanted and washes again and have dark crystals that remained and also a dark portion from washes that forms lighter crystals but dissolves later. This photo shows the lighter crystals starting to form but overnight it covered the entire bottom

What I’ll be doing with these dark crystals normally treated as impurities is after weighing them add lime and water to freebase then pull with ethyl acetate and see if it’ll crystallize as fumarate salt.

 

[modern]

I’m gonna make a guess that the dark crystals are different hydrate or different polymorph? Considering about 2/3 of the crude content being “impurities” or other alkaloids seems high but not impossible I guess.

I’ll report back whenever I get around to trying to use EtOAc

 

[bezevo]

so i read this a cpl times and it dosn't really say what your extracting from what plant .
so i see its under cactus .......my first clue .ha ha

but what kind of cactus , so on i'm interested in those details maybe i just missed it .

thanks for sharing interesting photos process .

 

[modern]

so i read this a cpl times and it dosn't really say what your extracting from what plant .
so i see its under cactus .......my first clue .ha ha

but what kind of cactus , so on i'm interested in those details maybe i just missed it .

thanks for sharing interesting photos process .

It was a mix of bridgesii that I cut back. 110g dry no special clones really just seed grown plants.

The strangest thing I’m experiencing which hopefully doing a mini cielo on the “impurities” will help me hopefully understand why there is a discrepancy between older papers which rarely pass 0.7% and recent extractions pull 2-3%. I get this but as crude salts but once “washed” always drops to that range. Even using xylene and hcl or other salt forms. I don’t quite understand why but do know the excess acid does pull more impurities.