HRID40967
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
The MCPBA (2.37 g, 10.6 mmol) was added to a solution of 1-bromo-3-(ethylthio)benzene (1.00 g, 4.80 mmol) in DCM (10 ml, 156 mmol) cooled to 0° C. The reaction was stirred for 1 h and then was diluted with water and extracted with ethyl acetate three times. The combined organic layers were dried with magnesium sulfate, filtered, and concentrated in vacuo. The resulting crude residue was purified by flash column chromatography with a hexane:ethyl acetate gradient to give 1-bromo-3-(ethylsulfonyl)benzene as a colorless oil 1.1 gm 92%, 1H NMR (300 MHz, CDCl3): δ□8.09(m, 1H), 7.85(d,1H), 7.78(d, 1H) 7.45(t,1H), 3.14(q, 2H), 1.25(t, 3H).
WORKUP
后处理
- extractionextracted with ethyl acetate three times
- dry with materialThe combined organic layers were dried with magnesium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe resulting crude residue was purified by flash column chromatography with a hexane