HRID1195454

反应详情

EQUATION

反应方程式

HRID 1195454 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Zinc amalgam (prepared by mixing zinc dust (25.0 g), mercuric chloride (2.5 g), concentrated hydrochloric acid (3 ml) and water (50 ml) together for 5 minutes, then decanting the aqueous solution) was added to a mixture of 4,7-dimethylindan-1-one (25.0 g, 156 mmole), acetic acid (50 ml), water (50 ml) and concentrated hydrochloric acid (100 ml). The mixture was refluxed with vigorous stirring for 12 hours, then cooled, poured into water and extracted with diethyl ether. The ether extract was washed successively with water, dilute aqueous sodium bicarbonate solution and water. Then dried over anhydrous sodium sulfate and concentrated. Purification by column chromatography over silica gel (eluant hexane) gave 4,7-dimethylindane (18.5 g, 81.4%) as an oil.

WORKUP

后处理

  1. customdecanting the aqueous solution)
  2. temperatureThe mixture was refluxed
  3. temperaturecooled
  4. extractionextracted with diethyl ether
  5. extractionThe ether extract
  6. washwas washed successively with water, dilute aqueous sodium bicarbonate solution and water
  7. dry with materialThen dried over anhydrous sodium sulfate
  8. concentrationconcentrated
  9. customPurification by column chromatography over silica gel (eluant hexane)