HRID546250

反应详情

EQUATION

反应方程式

HRID 546250 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
76 °C

PROCEDURE

实验过程

In a flask was placed 5-methyl-benzo[b]thiophene (3.64 g, 24.56 mmol) and carbon tetrachloride (75 mL). To the reaction mixture was then added N-bromosuccinimide (5.68 g, 31.92 mmol) and benzoyl peroxide (892 mg, 3.68 mmol) and it was the final solution was then heated at 76° C. for 6 h. After this time the reaction mixture was cooled to 0° C. in an ice bath and the solids were filtered off and the filterate was concentrated in vacuo and purified on an AnaLogix Intelliflash system (120 g column, 3% ethyl acetate/hexanes) to afford 5-bromomethyl-benzo[b]thiophene (5.27 g, 94%) as a yellow solid.

WORKUP

后处理

  1. customIn a flask was placed
  2. temperatureAfter this time the reaction mixture was cooled to 0° C. in an ice bath
  3. filtrationthe solids were filtered off
  4. concentrationthe filterate was concentrated in vacuo
  5. custompurified on an AnaLogix Intelliflash system (120 g column, 3% ethyl acetate/hexanes)