HRID841888

反应详情

EQUATION

反应方程式

HRID 841888 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. temperaturethe resulting mixture was refluxed for 5 h
  2. filtrationThe reaction mixture was filtered
  3. customevaporated
  4. customThe the remaining residue was purified by flash column chromatography on silica gel
  5. washeluted with hexane:ethyl acetate (7:3)