HRID9659

反应详情

EQUATION

反应方程式

HRID 9659 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A solution of 3-methyl-thiophene-2-carboxaldehyde (12.0 g) in chloroform (50 ml) was added drop-wise to bromine (5.1 ml) in chloroform over 30 minutes and then heated to 100° C. for 140 minutes. The reaction mixture was diluted with chloroform and washed with 10% aqueous sodium thiosulfate solution, saturated aqueous bicarbonate solution and water. The organic solution was dried over magnesium sulfate and concentrated. The product isolated after evaporation of the solvent was further purified by vacuum distillation (122° C., 4 mbar) to give the title compound as a green oil.

WORKUP

后处理

  1. washwashed with 10% aqueous sodium thiosulfate solution, saturated aqueous bicarbonate solution and water
  2. dry with materialThe organic solution was dried over magnesium sulfate
  3. concentrationconcentrated
  4. customThe product isolated
  5. customafter evaporation of the solvent
  6. distillationwas further purified by vacuum distillation (122° C., 4 mbar)