After one half botched attempt at the oxone route, cheese finally had complete success (with poor 30% yields) but the reason why things worked this time was becuase cheese buffered the oxone to get the Epoxide, instead of unbuffered to Glycol. Plus cheese learned that washing the Epoxide/Ketone with basic washes only works if the oil is suspended in toluene or another solvent of choice. Now the bisulphite test worked like a charm, 4 drops of light brown ketone solidified into a mass of buttery crystals int the test vial. The ketone appears to be relatively clean even without vacuum distilling it. Yields suffered due to impatience on cheese's half, not waiting long enough for washes to completely settle before tapping off with sep funnel, but cheese was happy to se them crystals form after 3 minutes of harsh aggravation. Thanks pickler, goiterjoe, Big R, locrian, VL_, and cheesegirl for putting up with cheese.
May De Sorce Bee Wit Chu-Always
Hey Big
R. Quick question, You know in Strike's book where you are making MDA from MD-Phenyl-2-Nitropropene, well after your last bit of boro is added you filtered through celite to remove the boride , then a quick wash with MeOH, then stripped of solvents with a vacuum and the residue is taken up with a dilute H2SO4 solution. OK here's the question and cheese thinks he knows the answer but wants things to be clear. Can a dilute H2SO4 solution be used to digest the aminated product from a cyano/ammonium acetate rxn as well? How come it's usually HCl that is called for with this step, will bothe types of acids work?