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
Formic acid (6.5 mL, 1 eq) was added to methyl 2-(3-fluoro-4-(methylthio)phenyl)propanoate (1 g, crude) and the mixture cooled to 0° C. Hydrogen peroxide (1.4 mL, 3 eq) was added drop wise at 0° C. and the reaction mixture was stirred overnight at room temperature. Progress of the reaction was monitored by TLC (20% ethyl acetate/hexane, Rf˜0.4). On completion of the reaction, the contents were cooled to 0° C., water was added and the mixture was extracted with ethyl acetate (2×25 mL). The combined extract was washed with NaHCO3 solution, dried over sodium sulfate and concentrated under reduced pressure to yield methyl 2-(3-fluoro-4-(methylsulfonyl)phenyl)propanoate as colorless thick liquid (1 g, crude). The crude product obtained was directly used for the next step.
WORKUP
后处理
- customOn completion of the reaction
- temperaturethe contents were cooled to 0° C.
- extractionthe mixture was extracted with ethyl acetate (2×25 mL)
- extractionThe combined extract
- washwas washed with NaHCO3 solution
- dry with materialdried over sodium sulfate
- concentrationconcentrated under reduced pressure