HRID732754
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
- 0 °C
PROCEDURE
实验过程
Dissolve 5-bromo-1,3-dihydro-benzo[c]thiophene (1.25 g, 5.79 mmol) in methanol (25 mL) and add oxone (10.7 g, 17.4 mmol). Stir the reaction mixture for 2 hours at 0° C. and then add a 1M aqueous sodium bisulfite solution (100 mL). Stir the reaction mixture for 10 minutes and add saturated NaHCO3 solution (200 mL). Extract the aqueous layer with CH2Cl2 (3×100 mL). Combine the organic layers and dry with Na2SO4, filter, concentrate and purify by flash column chromatography (silica gel, 0-5% MeOH/CH2Cl2) to give 930 mg of 5-bromo-1,3-dihydro-benzo[c]thiophene 2,2-dioxide 65%).
WORKUP
后处理
- stirringStir the reaction mixture for 10 minutes
- extractionExtract the aqueous layer with CH2Cl2 (3×100 mL)
- dry with materialCombine the organic layers and dry with Na2SO4
- filtrationfilter
- concentrationconcentrate
- custompurify by flash column chromatography (silica gel, 0-5% MeOH/CH2Cl2)