HRID1739428

反应详情

EQUATION

反应方程式

HRID 1739428 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionfurther thereto is added dropwise
  2. temperaturewith heating
  3. temperatureunder reflux over a period of one hour
  4. temperaturefor cooling
  5. temperaturecooling
  6. extractionThe mixture is extracted with chloroform
  7. washthe extract is washed
  8. customdried
  9. concentrationconcentrated
  10. customThe residue is recrystallized from isopropyl ether