Lysergic Acid Crystals Question

[Sleen]

Following the Jacobs Method of Alkaloid Hydrolysis - at the end:
The lysergic acid was dissolved in Warm MeOH and then cooled to 0 C and the crystals precipitated.

- White and grey crystals precipitated after allowing to sit at 0 C for 12 hours. The crystals were then filtered off.  Fortunately, the MeOH was put back in 0 C for 24 hours and again crystals precipitated - they were filtered.  This was repeated again with the same result, Although the amount has decreased each time. 
? - Is it normal that it should take so long for this precipitation to occur - from this, does it make more sense to leave the solution at 0 C for several days until all the precipitation has occured?

Second Question,
Using the CDI method for LA to LSD. What are the drawbacks to running this procedure with a small amount of LA other then working with small weights etc.
Example. If you have 0.1 grams of LA - can you still run the procedure or is there a size of reaction that limits this process?

Thanks anyone that can help!!

[hest]

? - Is it normal that it should take so long for this precipitation to occur - from this, does it make more sense to leave the solution at 0 C for several days until all the precipitation has occured

Yes, somtimes it will take 2-3 dayes for kompleet xtalisation, and this goes for all xtals, leave it in the fridge for 3 dayes and harvest.

Using the CDI method for LA to LSD. What are the drawbacks to running this procedure with a small amount of LA other then working with small weights etc.

That's right, small weights is the only problem.

[Sleen]

Thanks hest!

For small weights, all seem ok to weigh up except for the DEA, one drop weighs more then is needed, will an additional amount of DEA adversely effect the reaction?

If so - maybe use dilution with DMF or a smaller dropper?

Thanks again!