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
PROCEDURE
实验过程
To a methanol (2 ml) solution of 5-chloro-2-[[1-(2,5-difluorophenyl)-5-(methylsulfonyl)pentyl]thio]pyridine (100 mg, 0.25 mmol) was added a water (2 ml) solution of Oxone (potassium peroxymonosulfate compound, 2 KHSO5.KHSO4.K2SO4) (303 mg, 0.49 mmol) at 0° C. After shaking at room temperature for 22 hours, the reaction mixture was added with dichloromethane and the mixture was washed with water. The organic layer was dried over anhydrous sodium sulfate. After filtration, the filtrate was concentrated under reduced pressure. The residue was subjected to flash chromatography on a silica gel column, and the fraction obtained from the hexane:ethyl acetate=1:1 eluate was concentrated under reduced pressure, whereby the title compound (61 mg, 0.14 mmol, 56%) was obtained as a colorless foam.
WORKUP
后处理
- washthe mixture was washed with water
- dry with materialThe organic layer was dried over anhydrous sodium sulfate
- filtrationAfter filtration
- concentrationthe filtrate was concentrated under reduced pressure
- customthe fraction obtained from the hexane