HRID596681

反应详情

EQUATION

反应方程式

HRID 596681 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of finely ground 6-(3-allyl-4-hydroxyphenyl)-4,5-dihydro-3(2H)-pyridazinone (50g, 0.22 mole), epichlorohydrin (200 g, 2.2 mole) and piperidine (2g) was heated on a steam bath for 90 minutes. Evaporation under reduced pressure gave a viscous oil which was dissolved in dichloromethane and stirred for 10 minutes with dilute sodium hydroxide (500 ml). The organic phase was washed with water, dried and evaporated to an oil which slowly solidified. Addition of ethanol-ether gave 6[3-allyl-4-(2,3-epoxypropoxy)phenyl]-4,5-dihydro-3(2H)-pyridazinone (30g, 47%, m.p. 92.5°-95° C) which was recrystallised from aqueous ethanol to give the pure pyridazinone (m.p. 93.5°-95° C).

WORKUP

后处理

  1. temperaturewas heated on a steam bath for 90 minutes
  2. customEvaporation under reduced pressure
  3. customgave a viscous oil which
  4. washThe organic phase was washed with water
  5. customdried
  6. customevaporated to an oil which
  7. additionAddition of ethanol-ether