HRID649133
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
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
- temperatureafter which the mixture was heated
- temperatureunder reflux for 1 hour
- temperatureThe mixture was then cooled
- filtrationfiltered
- customthe filtrate was evaporated to dryness under reduced pressure
- customto give 3.11 g of crude crystals of the desired Compound No
- customThese were recrystallised from a 4:1 by volume mixture of hexane and benzene