反应详情

温度

80 °C

A solution of tert-butyl cyanoacetate (2.52 ml, 17.63 mmol), 3,4-dichlorobenzaldehyde (2.57 g, 14.69 mmol) and piperidine (0.145 ml, 1.469 mmol) in EtOH (50 ml) was allowed to stir at 80° C. for 15 hours, and then cooled to ambient temperature. A half volume of the solvent was evaporated, and 400 ml of water was added to the resulting mixture. The precipitated solid was collected and washed with 5% iPrOH/H2O (200 ml). The solid was dried under reduced pressure to give (E)-tert-butyl 2-cyano-3-(3,4-dichlorophenyl)acrylate (3.577 g); Retention time=1.61 minutes (condition A); MS (ES+)=315.1 (m+18).

1. temperaturecooled to ambient temperature
2. customA half volume of the solvent was evaporated
3. addition400 ml of water was added to the resulting mixture
4. customThe precipitated solid was collected
5. washwashed with 5% iPrOH/H2O (200 ml)
6. customThe solid was dried under reduced pressure