HRID84128

反应详情

EQUATION

反应方程式

HRID 84128 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 62.7 ml (500 mmol) of phenylethylamine, 70.4 ml (506 mmol) of triethylamine and 150 ml of dichloromethane was admixed dropwise at 0° C. with a solution of 109.2 g of 2-bromobenzoyl chloride in 50 ml of dichloromethane with good stirring at such a rate that the temperature did not exceed 30° C. Subsequently, the mixture was stirred at room temperature for a further 1 h. The colorless solid thus obtained was filtered off with suction, washed three times with 200 ml of dichloromethane and dried under reduced pressure. The yield at a purity of approx. 99.0% was 138.2 g (453 mmol), 90.7% of theory.

WORKUP

后处理

  1. customdid not exceed 30° C
  2. stirringSubsequently, the mixture was stirred at room temperature for a further 1 h
  3. customThe colorless solid thus obtained
  4. filtrationwas filtered off with suction
  5. washwashed three times with 200 ml of dichloromethane
  6. customdried under reduced pressure
  7. customThe yield at a purity of approx. 99.0%