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
CONDITIONS
反应条件
- 温度
- 110 °C
PROCEDURE
实验过程
100 g (0.43 mol) of (4-chlorophenyl)(4-hydroxyphenyl)methanone and 165 g (0.79 mol) of the 1-methylethyl ester of 2-bromo-2-methylpropanoic acid are introduced, under a nitrogen atmosphere, into a 3-necked round-bottomed flask equipped with a stirrer and a condenser. The reaction medium is heated to 110° C. and a solution of 50 g (0.36 mol) of potassium carbonate in 50 ml of demineralized water is then added slowly over a period of 20 minutes, with distillation taking place at 100° C. The distillate separates out into 2 phases. The lower phase is recycled into the reaction medium. After heating at 110°-112° C. for 1.5 h, the reaction medium is brought to 140° C. and a temperature of 140°-145° C. is maintained for 4 hours. The reaction medium is then cooled to about 90° C. and 210 ml of 80% isopropyl alcohol are added. The mixture is then left to cool for 12 h, with stirring, after which the suspension obtained is filtered at 0° C. The precipitate is washed with 4 times 200 ml of demineralized water and then recrystallized from propan-2-ol to give 119.5 g (yield=77%) of fenofibrate.
WORKUP
后处理
- customequipped with a stirrer and a condenser
- customat 100° C
- temperatureAfter heating at 110°-112° C. for 1.5 h
- customis brought to 140° C.
- temperaturea temperature of 140°-145° C. is maintained for 4 hours
- temperatureThe reaction medium is then cooled to about 90° C.
- waitThe mixture is then left
- temperatureto cool for 12 h
- customafter which the suspension obtained
- filtrationis filtered at 0° C
- washThe precipitate is washed with 4 times 200 ml of demineralized water
- customrecrystallized from propan-2-ol