myristicinaldehyde - 25-11-2017 at 04:47
I followed the following procedure from Vogel's 5 th edition. It worked almost exactly as described, even using multiple xylenes and shitty sulfuric
acid. One comment though- I heated for 4 hours on a water bath, not 15min.
When I tried to recrystalize from water, it does not want to come back out of solution! Any ideas? I fear hydrolysis, if I try to evaporate off more
water.
If I can get it back out of solution again, Ill make a writeup. It is a suprisingly easy reaction.
[Edited on 2017-11-26 by myristicinaldehyde]
myristicinaldehyde - 25-11-2017 at 12:56
It ended up crystalizing by itself when I took it *out* of the freezer. Hmmm.
unionised - 25-11-2017 at 13:04
That happens more often than you expect.
If you get the stuff cold enough the viscosity of the solution inhibits the crystal growth.