HRID26660

反应详情

EQUATION

反应方程式

HRID 26660 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

A mixture of 10.44 parts of 4-oxo-4H-1-benzopyran-3- carboxaldehyde and 5.4 parts of cyanoacetic acid are heated in an oil bath at 110° C., and to the mixture 25 volume parts of pyridine are added dropwise over about 30 seconds, after which time the whole mixture is further heated for 8 minutes. After cooling, the separated crystals are recovered by filtration, treated with activated carbon and recrystallized three times from ethanol. This procedure yields trans-3-(4-oxo-4H-1-benzopyran-3-yl)-acrylonitrile as pale-yellowish prisms. Melting point: 192°-194° C.

WORKUP

后处理

  1. temperatureafter which time the whole mixture is further heated for 8 minutes
  2. temperatureAfter cooling
  3. filtrationthe separated crystals are recovered by filtration
  4. additiontreated with activated carbon
  5. customrecrystallized three times from ethanol