HRID1739428
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of 2-bromo-4-(6,7-dimethoxy-2-methoxycarbonylmethylphthalazin-1(2H)-on-4-yl)pyridine (4.34 g) in tetrahydrofuran (20 ml) is added sodium borohydride (0.76 g), and further thereto is added dropwise with heating a mixture of methanol (3.2 ml) and tetrahydrofuran (5 ml) under reflux over a period of one hour. The reaction mixture is allowed to stand for cooling, and thereto is added water under ice-cooling. The mixture is extracted with chloroform, and the extract is washed, dried and concentrated. The residue is recrystallized from isopropyl ether to give 2-bromo-4-(6,7-dimethoxy-2-hydroxyethylphthalazin-1(2H)-on-4-yl)pyridine (3.08 g).
WORKUP
后处理
- additionfurther thereto is added dropwise
- temperaturewith heating
- temperatureunder reflux over a period of one hour
- temperaturefor cooling
- temperaturecooling
- extractionThe mixture is extracted with chloroform
- washthe extract is washed
- customdried
- concentrationconcentrated
- customThe residue is recrystallized from isopropyl ether