2-chloro-2-methylpropiononitrile synthesis
- Product Name:2-chloro-2-methylpropiononitrile
- CAS Number:3331-60-0
- Molecular formula:C4H6ClN
- Molecular Weight:103.55
Yield:-
Reaction Conditions:
with phosgene;Cyanex 923 in o-xylene at 95 - 107; for 5.67 h;
Steps:
4 Chloroisobutyronitrile
150 g of o-xylene and 10.4 g (0.03 mol) of Cyanex 923 are initially introduced into a phosgenation apparatus with attached carbonic acid condenser and heated. At from 97 to 103° C., 20 g of phosgene are gassed in over the course of 10 minutes. Thereafter, over the course of 5 hours, 67 g (0.8 mol) of acetone cyanohydrin and a further 72 g (total=92 g or 0.93 mol) of phosgene are added in parallel. The internal temperature is maintained at between 95 and 103° C. throughout. After a post-reaction of 30 minutes at 107° C., excess phosgene is stripped out using N2 at 50° C. for 2 h. The discharge of 209.5 g comprises 42% of methacrylonitrile (by elimination of HCl) and 51 % of chloroisobutyronitrile and is fractionally distilled on a 30 cm Vigreux column. Since the HCl is eliminated thermally during the distillation, isolation is unsuccessful.
References:
BASF Aktiengesellschaft US6353127, 2002, B1 Location in patent:Page column 4-5
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