swid did two attempts:
1. 100ml EtOH
101ml BA
79ml NE
20ml n-But.amin
refluxed 2 hours at 83° C.
Result: one layer of red/orange layer. Put this in
the freezer: milky white upper layer appeared and
sucked away.
orange/red layer cooled again down to -10°C and then
swirled to bring it in contact with air:
the whole mass crystallized in a few seconds.
re-X with IPA gave a beaker full of near white
sparkling beauties
2. no solvent was used
49 ml BA
38 ml NE
6 ml n-Butyla.
refluxed for 2 hours at 100°C
result: water layer over a deep orange oil layer.
water drained away with sep. funnel.
oil cooled again to -10°C, swirled to bring it in
contact with air and -again- the whole shebang
crystallized in a few seconds.
> re-X with IPA > some result as in the first attempt
yield is over 80% in 1. + 2.
the trick is: to cool it down in the freezer and then swirl it with a glas rod to bring air in the oil.
dean-stark trap was not necessary
greez