Guys, I have a few questions, and I guess some of you chemical killers can help me out.
First, I am trying to hydrolyse ergot tartrate that is 100% white, and in KOH solution continues white. I have a pharmacopeia that says ergotamine can be either white or yellow.
I am guessing the yellow one shulgin and everyone else mentions is the "other" type of ergotamine. What I want to ask is: has anyone ever worked w/ white ET? does it continue white in KOH solution? What I notice is that it turns yellow ( maybe greenish-yellow ) under UV flashes.
Well, I purify my product and I usually get a little over what I'm supposed to ( maybe 10% in average) which I find strange.
Then I proceed to the POCL3 method, I heat up, add everything, and voilá. I dry my solvent after washing and when I dissolve in methanol, I see that not EVERYTHING is dissolved. Then I add the maleic acid (20% in methanol) and very little crystalyzes. I don't get needles, but some sparse dust and I figure it's not even worth filtering.
I don;t plan to give up yet, so I dillute this whole thing in water, estimating that I have something like one gram of good LSD. I take it and I trip some. I give it to friends, and they say it's mild, but clean and the feeling is very pleasant.
My conclusion is: I DID get lsd, but why is it not crystalysing? I would like to remind that my lab is completely dark w/ blackout curtains, 20 square meters big w/ a 30000 BTU air conditioner and an extra dehumidifier, all My solvents(methanol and chloroform are HPLC, and I have an oven in which I dry all my glassware before use.
My reflux column is about -8C cold and a generous nitrogen flow (and bubbling) is present at all times in my reactions.
I have thermostats for my oil baths, the only thing I am guessing is not 100% is my vacuum pump, its giving me something like 30-40mm vacuum. Could this be so important?
I am waiting 2-3 days for drying solvents. Also, when I dry the LSD freebase, I don't get crystals, I get some sort of a plate, feels hard, but definitely is not a bunch of crystals.
Guys, help me out. I need to get some reasonable yield here.
(Oh, the ET source is pretty reliable) (and I DID get a very strong trip once, when I licked my instruments)
thanks for the time and knowledge