HRID929376

反应详情

EQUATION

反应方程式

HRID 929376 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To N-methyl maleimide (0.5 g, 4.5 mmol) in methanol (22.5 mL) was added bromine (0.52 mL, 10 mmol) dropwise. The reaction mixture was stirred at room temperature for 24 hours. Solvent was removed in vacuo and the reaction mass was dissolved in tetrahydrofuran (20 mL) and triethylamine (0.8 mL, 5.85 mmol) added, then stirred for 24 hours at room temperature. The material was purified by flash chromatography on silica gel (petroleum ether: ethyl acetate, 7:3) to afford a pale white powder (0.761 g, 4.0 mmol) in 89% yield.

WORKUP

后处理

  1. customSolvent was removed in vacuo
  2. dissolutionthe reaction mass was dissolved in tetrahydrofuran (20 mL)
  3. stirringstirred for 24 hours at room temperature
  4. customThe material was purified by flash chromatography on silica gel (petroleum ether: ethyl acetate, 7:3)