HRID2040924

反应详情

EQUATION

反应方程式

HRID 2040924 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

An amount of 54.25 g (0.529 mol) of 2,2-difluoro-1-chloroethane, 9.1 g (0.066 mol) of potassium carbonate and 50 g (0.264 mol) of potassium phthalimide are dissolved in 237 g of N,N-dimethylformamide. The reaction mixture is stirred in an autoclave under pressure at 120° C. for 12 h. After the end of the reaction, cooling is carried out to ambient temperature and the solvent is exhaustively removed under vacuum. The remaining residue is treated with 250 ml of water and the solid is filtered off. The filter residue is washed twice with water and the product is dried under vacuum. An amount of 55.5 g of 2-(2,2-difluoroethyl)-1H-isoindole-1,3(2H)-dione with a purity of 96.5% is obtained. This corresponds to a yield of 95.8% of theory.

WORKUP

后处理

  1. customAfter the end of the reaction
  2. temperaturecooling
  3. customis carried out to ambient temperature
  4. customthe solvent is exhaustively removed under vacuum
  5. additionThe remaining residue is treated with 250 ml of water
  6. filtrationthe solid is filtered off
  7. washThe filter residue is washed twice with water
  8. customthe product is dried under vacuum