HRID333736
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 a suspension of methyl 5-methoxy-4-oxo-1-phenyl-1,4-dihydropyridazine-3-carboxylate (39.04 g) in methanol (663 mL) was added dropwise 1N sodium hydroxide (300 mL) with stirring under ice-cooling, and the mixture was allowed to warm to room temperature and stirred for 1 hr. 1N Hydrochloric acid (300 mL) was added dropwise with stirring under ice-cooling, and the mixture was stirred at the same temperature for 1 hr. The precipitated crystals were collected by filtration, washed successively with water, ethanol/diisopropyl ether (1/2), and diisopropyl ether, and dried to give the title compound (36.1 g) as pale-yellow crystals.
WORKUP
后处理
- temperaturecooling
- stirringstirred for 1 hr
- stirringwith stirring under ice-
- temperaturecooling
- stirringthe mixture was stirred at the same temperature for 1 hr
- filtrationThe precipitated crystals were collected by filtration
- washwashed successively with water, ethanol/diisopropyl ether (1/2), and diisopropyl ether
- customdried