HRID328308

反应详情

EQUATION

反应方程式

HRID 328308 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

Thousand gram of 4-n-pentanoylbiphenyl, 2 l of diethylene glycol and 564 g of potassium hydroxide were introduced into a 5 l three neck flask and warmed with stirring to give a uniform solution at about 80° C, which was then cooled to about 50° C, followed by adding 738 ml of hydrazine hydrate, heating with stirring, distilling off low boiling fractions (mainly water) until the temperature of the reaction mixture reached 185° C, heating under reflux at 185°-190° C for 4 hours, cooling to room temperature, adding 1.5 l of water and 400 ml of hexane, stirring, washing hexane layer with aqueous solution of sodium chloride, and distilling, to give 659 g of 4-n-pentylbiphenyl (b.p. 166°-167°/6 mmHg) (Yield 70%).

WORKUP

后处理

  1. temperaturewarmed
  2. customto give a uniform solution at about 80° C
  3. temperatureheating
  4. stirringwith stirring
  5. distillationdistilling off low boiling fractions (mainly water) until the temperature of the reaction mixture
  6. customreached 185° C
  7. temperatureheating
  8. temperatureunder reflux at 185°-190° C for 4 hours
  9. temperaturecooling to room temperature
  10. additionadding 1.5 l of water and 400 ml of hexane
  11. stirringstirring
  12. washwashing hexane layer with aqueous solution of sodium chloride
  13. distillationdistilling