HRID278403
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
1.39 g of 5-acetonyl-3-methylisoxazole, 1.68 g of 3,4-dihydro-6-methyl-2H-pyran-2-one and 3.42 g of cecium carbonate were added to 20 ml of acetonitrile to heat at reflux for 3 hours. After returning to room temperatrure, the reaction solution was poured into 100 ml of ice water with hydrochloric acid added, and extracted with ethyl acetate. The organic layer was washed with water and then with saturated salt water, and dried over magnesium sulfate. The solvent was concentrated under reduced pressure. The obtained crude product was purified on silica gel column chromatography to give 2.03 g of the title compound as a colorless viscous liquid.
WORKUP
后处理
- temperatureto heat
- temperatureat reflux for 3 hours
- additionadded
- extractionextracted with ethyl acetate
- washThe organic layer was washed with water
- dry with materialwith saturated salt water, and dried over magnesium sulfate
- concentrationThe solvent was concentrated under reduced pressure
- customThe obtained crude product
- customwas purified on silica gel column chromatography