HRID1904353

反应详情

EQUATION

反应方程式

HRID 1904353 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of the product of Step A, 5 ml of pyridine and 1 ml of methanesulfonyl chloride was stirred for 31/2 hours and was then diluted with N hydrochloric acid. The mixture was extracted with methylene chloride and the organic phase was washed with water, dried and evaporated to dryness under reduced pressure. The 677 mg of residue was chromatographed over silica and was eluted with a 7-3 mixture of hexane-ethyl acetate to obtain 410 mg of 6-(1,1-dimethylethoxy)-5-methylsulfonyloxy-4,4-dimethyl-tetrahydro-pyr-2-one melting at 64° C.

WORKUP

后处理

  1. extractionThe mixture was extracted with methylene chloride
  2. washthe organic phase was washed with water
  3. customdried
  4. customevaporated to dryness under reduced pressure
  5. customThe 677 mg of residue was chromatographed over silica
  6. washwas eluted with a 7-3 mixture of hexane-ethyl acetate