HRID1461587

反应详情

EQUATION

反应方程式

HRID 1461587 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customIn a four-necked flask of 200 ml provided with a stirrer
  2. additionto which was added
  3. temperaturewas maintained at 15° C.
  4. stirringwith stirring
  5. temperatureAfter the liquid temperature was raised to 25° C.
  6. waitfurther the stirring was made for 5 minutes
  7. customThe water phase was separated
  8. washwashed with an aqueous solution of 40 g of 5% sodium hydroxide and further with water three times
  9. dry with materialThe solution was dried on magnesium sulfate anhydride and benzene
  10. customwas removed off under vacuum