HRID84128
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customdid not exceed 30° C
- stirringSubsequently, the mixture was stirred at room temperature for a further 1 h
- customThe colorless solid thus obtained
- filtrationwas filtered off with suction
- washwashed three times with 200 ml of dichloromethane
- customdried under reduced pressure
- customThe yield at a purity of approx. 99.0%