HRID532466

反应详情

EQUATION

反应方程式

HRID 532466 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

4-bromo-2-fluoroaniline (10.0 g, 52.62 mmol, 1.0 eq), sodium methansulfinate (9.5 g, 1.5 eq), copper(I) iodide (1.0 g, 0.1 eq), L-Proline (1.2 g, 0.2 eq) and sodium hydroxide (0.4 g, 0.2 eq) were placed in a sealed tube, and dimethylsulfoxide (100 mL) was added thereto. The reaction mixture was stirred at 90° C. for 24 hours. After completion of the reaction, the reaction mixture was cooled to room temperature and water was added thereto, followed by extraction three times with ethyl acetate. The extract was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The resulting compound was purified using column chromatography (MC:MeOH=50:1) to obtain the title compound (9.9 g).

WORKUP

后处理

  1. customAfter completion of the reaction
  2. temperaturethe reaction mixture was cooled to room temperature
  3. extractionfollowed by extraction three times with ethyl acetate
  4. dry with materialThe extract was dried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe resulting compound was purified