HRID1906663
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
A suspension of 6-[4-(3-bromopropionamido)phenyl]-5-methyl-4,5-dihydro-3(2H)-pyridazinone (120 g, 0.355 mol) and benzylamine (152 g, 1.47 mol) in n-propanol (800 ml) was stirred under reflux for 16 hours. The reaction mixture was filtered whilst hot and white solid was collected, which was washed with ether to remove excess benzylamine. The crude material was boiled with ethanol (300 ml) for 2 hours; the mixture was cooled and filtered. The resulting white solid was washed with ether and dried to give 6-[4-(3-benzylaminopropionamido)phenyl]-5-methyl-4,5-dihydro-3(2H)-pyridazinone (114 g, 88%) as the hydrobromide salt m.p. 279°-285° C.
WORKUP
后处理
- temperatureunder reflux for 16 hours
- filtrationThe reaction mixture was filtered whilst hot and white solid
- customwas collected
- washwhich was washed with ether
- customto remove excess benzylamine
- temperaturethe mixture was cooled
- filtrationfiltered
- washThe resulting white solid was washed with ether
- customdried