HRID47078

反应详情

EQUATION

反应方程式

HRID 47078 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 60 mg (0.0025 mole) of sodium hydride in 7 ml of toluene was added 4.32 ml (0.025 mole) of ethyl benzoyl acetate. After several minutes a solution was obtained to which was added 2.41 ml (0.025 mole) of cyclohexenone. The reaction was stirred 36 hrs. at room temperature and then added to 25 ml 1 N hydrochloric acid--25 ml saturated sodium chloride--150 ml ether. The ether extract was dried over magnesium sulfate and evaporated to an oil. This crude oil was purified via column chromatography on 300 g of silica gel eluted with 50% ether--pentane to yield 4.8 g (67%) of the title compound as an oil.

WORKUP

后处理

  1. customAfter several minutes a solution was obtained to which
  2. extractionThe ether extract
  3. dry with materialwas dried over magnesium sulfate
  4. customevaporated to an oil
  5. customThis crude oil was purified via column chromatography on 300 g of silica gel
  6. washeluted with 50% ether