HRID926964
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturemaintaining the same temperature
- customovernight
- customat room temperature
- customThe solvent was evaporated under vacuum
- dissolutionthe residue was dissolved in dichloromethane
- washThe organic layer was washed with Na2S2O3 20%
- dry with materialdried over anhydrous Na2SO4
- concentrationconcentrated to dryness