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
- 10 °C
PROCEDURE
实验过程
In a four-necked flask of 200 ml provided with a stirrer was charged 33.7 g of an aqueous solution of 30% potassium hydroxide, to which was added a mixture of 22.1 g of 95% 1-phenylcyclohexyl hydroperoxide and 30 g of benzene while the liquid temperature was maintained at 10° C. with stirring. Furthermore, 19.1 g of neodecanoyl chloride was added dropwise over 7 minutes while the liquid temperature was maintained at 15° C. with stirring. After the liquid temperature was raised to 25° C. and the stirring was continued for 2 hours, 40 g of cold water was added and further the stirring was made for 5 minutes. The water phase was separated and washed with an aqueous solution of 40 g of 5% sodium hydroxide and further with water three times. The solution was dried on magnesium sulfate anhydride and benzene was removed off under vacuum to obtain 24.0 g of a desired compound as a light yellow liquid. This compound had an active oxygen amount of 4.20%, a purity of 91% through calculation and a yield of 63 mol %.
WORKUP
后处理
- customIn a four-necked flask of 200 ml provided with a stirrer
- additionto which was added
- temperaturewas maintained at 15° C.
- stirringwith stirring
- temperatureAfter the liquid temperature was raised to 25° C.
- waitfurther the stirring was made for 5 minutes
- customThe water phase was separated
- washwashed with an aqueous solution of 40 g of 5% sodium hydroxide and further with water three times
- dry with materialThe solution was dried on magnesium sulfate anhydride and benzene
- customwas removed off under vacuum