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.
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.
