At about pH 9 you'll start to see amber oil fall ems the goods and its a damn pretty sight to see.
After 48-72 hours, take the balloon off and distill off the methanol.
Ketone can only be recycled once, after that it degrades.Reitz Reductive Aminations of Carbonyl Compounds with Borohydride and Borane Reducing Agents in Organic Reactions, 2002, John Wiley and Sons.Reductive amination by NaBH3CN is sometimes done in the presence of certain Lewis acids (ex.MDA by reductive amination with NaBH3CN.Once the contents of the flask have cooled ( 40C carefully add 2L of 10 HCL(roughly 660ml muriatic and 1340ml distilled H2O.) Add slowly and make sure fizzing doesnt get out of hand or you will be wearing it!The meth cook will sample the meth and continue his work in an energized manner for many more hours or days.Its possible to use the familiar reducing agent sodium borohydride (NaBH4) for this process.I have never seen this to be true."Cyanohydridoborate Anion as a Selective Reducing Agent".Stir it a little and quickly add it to the 5L flask.
Reminder: Alkylation of Amines Is Rarely The Answer.
The SM (1 equiv) and dry acetone (5 equiv).
The aldehyde or ketone is typically prestirred with the amine in the presence of the Lewis acid, then treated with NaBH3CN.
Heres the mechanism for imine formation, in case youve forgotten.
There are two other commonly used reductants for reductive amination: sodium cyanoborohydride (NaBH3CN) and sodium tri-acetoxyborohydride (NaBH(OAc)3 ).Reductive amination using sodium cyanoborohydride address this issue properly.Take the dcm/freebase oil and freeze till ya ready to xtallize.Note: during the 2-3 day wait, make up about 2L of saturated NaOH (lye) solution and freeze.For research purposes the place to start for primary literature is the Merck Index.We could have done the first reductive amination with benzaldehyde first, and acetone second, and still obtained the same product.