HRID232608

反应详情

EQUATION

反应方程式

HRID 232608 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

To a stirred solution of NaOEt (from 0.69 g sodium), in ethanol (25 ml) at reflux, was added over 5 minutes a mixture of 3,5-dichlorophenylacetonitrile (9.3 g) and ethyl acetate (3.3 g) in dry dimethoxyethane (10 ml). After stirring at reflux for 4 hours, the mixture was cooled on ice, acidified with acetic acid, poured into cold water and extracted with dichloromethane. The combined extracts were washed with water and concentrated to give an oil. Trituration with hexane gave 2-(3,5-dichlorophenyl)-3-oxobutyronitrile as a colourless solid (4.15 g).

WORKUP

后处理

  1. additionwas added over 5 minutes
  2. temperatureat reflux for 4 hours
  3. temperaturethe mixture was cooled on ice
  4. extractionextracted with dichloromethane
  5. washThe combined extracts were washed with water
  6. concentrationconcentrated
  7. customto give an oil