HRID1638144
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 solution of tetrahydrothiopyran-4-one-3-carboxylic acid, allyl ester (Example 4, step A) (2.3 g, 11.5 mmol) in 100 mL dry chloroform at room temperature was added activated manganese dioxide (10 g, 115 mmol) and the resulting mixture was refluxed for 5 h. The reaction mixture was filtered and evaporated. The the remaining residue was purified by flash column chromatography on silica gel eluted with hexane:ethyl acetate (7:3) to give 2,3-dihydrothiopyran-4-one-3-carboxylic acid, allyl ester (0.988 g).
WORKUP
后处理
- temperaturethe resulting mixture was refluxed for 5 h
- filtrationThe reaction mixture was filtered
- customevaporated
- customThe the remaining residue was purified by flash column chromatography on silica gel
- washeluted with hexane:ethyl acetate (7:3)