HRID649133

反应详情

EQUATION

反应方程式

HRID 649133 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 50 ml of dry benzene were added 2.51 g of 6-(3-bromophenyl)-3(2H)-pyridazinone, 0.45 g of paraformaldehyde and 1 ml of thionyl chloride, after which the mixture was heated under reflux for 1 hour. The mixture was then cooled and filtered, and the filtrate was evaporated to dryness under reduced pressure, to give 3.11 g of crude crystals of the desired Compound No. 5. These were recrystallised from a 4:1 by volume mixture of hexane and benzene, to give 2.0 g of pure Compound No. 5, in the form of white needles melting at 135°-137° C.

WORKUP

后处理

  1. temperatureafter which the mixture was heated
  2. temperatureunder reflux for 1 hour
  3. temperatureThe mixture was then cooled
  4. filtrationfiltered
  5. customthe filtrate was evaporated to dryness under reduced pressure
  6. customto give 3.11 g of crude crystals of the desired Compound No
  7. customThese were recrystallised from a 4:1 by volume mixture of hexane and benzene