HRID973807

反应详情

EQUATION

反应方程式

HRID 973807 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

Methyl 3-cyanocinnamate (42 pw) is added to a mixture of trichloroacetonitrile (194.4 pw) and aluminum bromide (7.2 pw) in the absence of moisture and at about 25° C. Hydrogen chloride is then introduced over a period of 3 hours with stirring, while keeping the temperature constant. Stirring is discontinued, and the mixture is allowed to react further overnight. In this step, too, a constant temperature of 25° C. is maintained. The solidified mixture is dissolved in 800 pw of dichloromethane, washed with water, and the organic phase is dried over sodium sulfate. Evaporation of the solvent gives a white residue, which is recrystallized from methanol or benzene.

WORKUP

后处理

  1. stirringStirring
  2. customto react further overnight
  3. washwashed with water
  4. dry with materialthe organic phase is dried over sodium sulfate
  5. customEvaporation of the solvent
  6. customgives a white residue, which
  7. customis recrystallized from methanol or benzene