反应详情

温度

0 °C

390 g of 4-bromomethylcinnamonitrile are suspended in 600 ml of trimethylphosphite and the suspension is added in portions to 250 ml of well stirred trimethylphosphite of 90° C., such that the strongly exothermic reaction can be kept under control. Excess trimethylphosphite is then distilled off under a water jet vacuum and 330 ml of toluene and 660 ml of hexane are added to the residue, which is cooled to 0° C. The crystallised product is filtered with suction and vacuum dried at 50° C., affording 427 g of 4-(dimethoxyphosphorylmethylphenyl)cinnamonitrile with a melting point of 98°-101° C.

1. distillationExcess trimethylphosphite is then distilled off under a water jet vacuum and 330 ml of toluene and 660 ml of hexane
2. additionare added to the residue, which
3. filtrationThe crystallised product is filtered with suction and vacuum
4. customdried at 50° C.