HRID1608022

反应详情

EQUATION

反应方程式

HRID 1608022 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 7 g of 5,6-epoxy-4,4-dimethyl-tetrahydro-pyr-2-one, 35 ml of isopropanol and 350 mg of p-toluene sulfonic acid was stirred at room temperature for 23 hours and was diluted with water. The mixture was extracted with methylene chloride and the combined extracts were washed with aqueous saturated sodium bicarbonate solution, was dried and evaporated to dryness under reduced pressure. The 9.18 g of residue was chromatographed over silica and was eluted with a 1-1 mixture of hexane-ethyl acetate to obtain 2.597 g of dl 6-isopropoxy-5-hydroxy-4,4-dimethyl-tetrahydro-pyr-2-one melting at 50° C.

WORKUP

后处理

  1. extractionThe mixture was extracted with methylene chloride
  2. washthe combined extracts were washed with aqueous saturated sodium bicarbonate solution
  3. customwas dried
  4. customevaporated to dryness under reduced pressure
  5. customThe 9.18 g of residue was chromatographed over silica
  6. washwas eluted with a 1-1 mixture of hexane-ethyl acetate