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
A mixture consisting of 354 mg (1.58 mmol) of 5,7-dihydroxy-2-methylthiochromone, 1.09 g (7.90 mmol) potassium carbonate, 0.79 ml (7.90 mmol) isopropyl iodide, and 20 ml acetone was refluxed overnight. Then, 2.95 ml (47.4 mmol) methyl iodide was added, and the mixture was further refluxed overnight. Water was added to the solution thus reacted. The product was extracted twice with ethyl acetate. The organic layer was washed with saturated salt water and dried over sodium sulfate anhydride. The solvent was distilled out under reduced pressure. The resulting crude product was purified by flash column chromatography (hexane: ethyl acetate =1:3-1:6), whereby 228 mg of 7-isopropoxy-5-methoxy-2-methylthiochromone was obtained (yield: 52%).
WORKUP
后处理
- temperaturewas refluxed overnight
- temperaturethe mixture was further refluxed overnight
- customthus reacted
- extractionThe product was extracted twice with ethyl acetate
- washThe organic layer was washed with saturated salt water
- dry with materialdried over sodium sulfate anhydride
- distillationThe solvent was distilled out under reduced pressure
- customThe resulting crude product was purified by flash column chromatography (hexane: ethyl acetate =1:3-1:6)