HRID590973

反应详情

EQUATION

反应方程式

HRID 590973 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Aluminium chloride (0.26 g, 1.98 mmol) was added to a solution of 2,4-dibromothiophene (0.30 g, 1.24 mmol) and ethyl chlorooxoacetate (0.19 g, 1.36 mmol) in dichloromethane (10 mL) previously cooled with an ice bath. The reaction mixture was stirred at room temperature for 45 minutes, poured into ice water and extracted with dichloromethane (2×20 mL). The organic layer was dried over sodium sulfate, filtered and concentrated in vacuo to provide ethyl 2-(3,5-dibromothiophen-2-yl)-2-oxoacetate (0.42 g, 1.24 mmol, 100%) as a yellow oil.

WORKUP

后处理

  1. temperaturepreviously cooled with an ice bath
  2. extractionextracted with dichloromethane (2×20 mL)
  3. dry with materialThe organic layer was dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo