HRID1624857

反应详情

EQUATION

反应方程式

HRID 1624857 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of 1 g (5.3 mmoles) of 3-(3,4-dimethoxyphenyl)propanenitrile in 42 mL of DMF is cooled to 0° C. To the resulting solution there is added, little by little, 0.93 g of NBS (5.2 mmoles, 1 eq.). After stirring for 30 minutes at 0° C., the reaction mixture is brought back to ambient temperature and stirred for two hours. It is then hydrolysed using 170 mL of water and extracted twice with 130 mL of ethyl acetate. The organic phases are collected and then washed, first with saturated aqueous Na2S2O5 solution and then with water. After evaporating off the solvent under reduced pressure, 1.29 g of a colourless oil which crystallises into a white solid are obtained.

WORKUP

后处理

  1. additionTo the resulting solution there is added
  2. customis brought back to ambient temperature
  3. stirringstirred for two hours
  4. extractionextracted twice with 130 mL of ethyl acetate
  5. customThe organic phases are collected
  6. washwashed, first with saturated aqueous Na2S2O5 solution
  7. customAfter evaporating off the solvent under reduced pressure, 1.29 g of a colourless oil which
  8. customcrystallises into a white solid
  9. customare obtained