HRID2269671

反应详情

EQUATION

反应方程式

HRID 2269671 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A slurry of 1.11 g (5 mmole) of 4-bromo-3-methyl-2-thiophenecarboxylic acid, 0.44 mL (6 mmole) of thionyl chloride, 5 drops of DMF, and 10 mL of 1,2-dichloroethane was heated at 80° C. for 1.5 h. The clear solution was cooled and concentrated on a roto-evaporator. The residue was dissolved in 5 mL of 1,2-dichloroethane and reconcentrated on a roto-evaporator to give 1.2 g of a tan solid, 97% pure (GC area). This acid chloride was used without further purification.

WORKUP

后处理

  1. temperatureThe clear solution was cooled
  2. concentrationconcentrated on a roto-evaporator
  3. dissolutionThe residue was dissolved in 5 mL of 1,2-dichloroethane
  4. customreconcentrated on a roto-evaporator