HRID1461538
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
4-Benzoyloxy-1-dimethylamino-1-hexene-3,5-dione (24.75 g, 90 mmol) is refluxed in 180 ml of acetic acid for 90 minutes. The reaction mixture is concentrated at 30°-35° C. on a rotary evaporator, the residue is dissolved in 200 ml of dichloromethane and washed twice with 100 ml of saturated sodium bicarbonate solution each time. The organic phase is dried over magnesium sulphate, concentrated on a rotary evaporator and gives 20.11 g (97.1%) of 3-benzoyloxy-2-methyl-4-pyrone. Content 86%, m.p. 106°-110° C.
WORKUP
后处理
- concentrationThe reaction mixture is concentrated at 30°-35° C. on a rotary evaporator
- dissolutionthe residue is dissolved in 200 ml of dichloromethane
- washwashed twice with 100 ml of saturated sodium bicarbonate solution each time
- dry with materialThe organic phase is dried over magnesium sulphate
- concentrationconcentrated on a rotary evaporator