HRID926964

反应详情

EQUATION

反应方程式

HRID 926964 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-40 °C

PROCEDURE

实验过程

Methyl phenyl sulfoxide (21.644 g, 154.4 mmol) was dissolved in anhydrous pyridine (27.4 mL, 2.2 eq) and dry acetonitrile (100 mL). The solution was cooled to −40° C. under an argon atmosphere. A solution of bromine (49.4 g, 2 eq) in dry acetonitrile (50 mL) was added slowly, maintaining the same temperature. The mixture was stirred at −40° C. for 1 h and then overnight at room temperature. The solvent was evaporated under vacuum and the residue was dissolved in dichloromethane. The organic layer was washed with Na2S2O3 20%, dried over anhydrous Na2SO4 and concentrated to dryness.

WORKUP

后处理

  1. temperaturemaintaining the same temperature
  2. customovernight
  3. customat room temperature
  4. customThe solvent was evaporated under vacuum
  5. dissolutionthe residue was dissolved in dichloromethane
  6. washThe organic layer was washed with Na2S2O3 20%
  7. dry with materialdried over anhydrous Na2SO4
  8. concentrationconcentrated to dryness