HRID1985740

反应详情

EQUATION

反应方程式

HRID 1985740 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Chloroacetylacetone 8 g (59.4 mmol) is dissolved in 70 ml of glacial acetic acid and ammonium acetate 13.7 g (178.2 mmol) is then added and the mixture is refluxed for 4 hours. The solution is cooled, brought to pH 5 and extracted into ether; the organic layer is dried over Na2SO4 and concentrated to dryness in vacuo. The residue is purified by column chromatography on silica gel using 8:2 hexane:ethyl acetate as eluent. The 2,4-dimethyl-5-acetyloxazole is obtained as orange needles (2.2 g, 27%).

WORKUP

后处理

  1. temperaturethe mixture is refluxed for 4 hours
  2. temperatureThe solution is cooled
  3. extractionextracted into ether
  4. dry with materialthe organic layer is dried over Na2SO4
  5. concentrationconcentrated to dryness in vacuo
  6. customThe residue is purified by column chromatography on silica gel using 8:2 hexane