HRID1427908

反应详情

EQUATION

反应方程式

HRID 1427908 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

A mixture of 5-chloro-2-fluoro-4-methyl-N-(methylsulfonyl)benzamide (0.8 g, 3.0 mmol), N-bromosuccinimide (1.6 g, 9.0 mmol) and azodiisobutyronitrile (16 mg, 0.09 mmol) in 1,2-dichloroethane (20 mL) was stirred at 90° C. for 16 hrs. The reaction was quenched with Na2S2O3 (10 mL, 10%), extracted with 1,2-dichloroethane (20 mL×3), dried over anhydrous Na2SO4, concentrated and the residue was used in next step without further purification (1.1 g, crude). LCMS (ESI) m/z: 342.0 [M+H]+.

WORKUP

后处理

  1. customThe reaction was quenched with Na2S2O3 (10 mL, 10%)
  2. extractionextracted with 1,2-dichloroethane (20 mL×3)
  3. dry with materialdried over anhydrous Na2SO4
  4. concentrationconcentrated
  5. customthe residue was used in next step without further purification (1.1 g, crude)