From: Jacob Zabicky (zabicky$##$bgumail.bgu.ac.il)
Date: Thu Jun 10 1999 - 06:39:21 EDT
>Do you think the chloro nitroso product
>left dry in the bottom of the hot distillation flask
>would decompose or even explode?
>Jerry Morine
Hello Jerry,
It's generally no good policy to distill the products of organic syntheses
to dryness. You frequently get a dark tar, and sometimes carbonization is
quite extensive. Nitroso compounds should be more stable than the analogous
nitro compounds. I'm not sure what to expect from the geminal nitroso and
chloro groups as far as thermal stability goes. try to heat a few drops of
your "elixir" in a hood and see what's left. Your probably have enough to
run an IR or even an NMR. If the chloro-nitroso survives, then the think to
do would be a three stage distillation: at about 20 torr you get rid of the
solvents, say in a Rotavapor controption, then, at a couple of torrs (using
a pressure stabilizer) you can distill off ethyl malonate; then reduce the
pressure again and start distilling the chloro-nitoso compound (using a
pressure stabilizer) discarding the first part of the distillation. If you
have a small molecular still, it may be very helpful for the last stage.
All the best,
Jacob
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