HRID1985740
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe mixture is refluxed for 4 hours
- temperatureThe solution is cooled
- extractionextracted into ether
- dry with materialthe organic layer is dried over Na2SO4
- concentrationconcentrated to dryness in vacuo
- customThe residue is purified by column chromatography on silica gel using 8:2 hexane