HRID1639770

反应详情

EQUATION

反应方程式

HRID 1639770 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of lithium aluminum hydride (1.09 g, 28.7 mmol) in tetrahydrofuran (60 mL) was added a solution of methyl 5-bromo-2-ethyl-2H-indazole-4-carboxylate (2.03 g, 7.17 mmol) in tetrahydrofuran (15 mL) under nitrogen atmosphere at 0° C., and the mixture was stirred at room temperature for 50 hr. Sodium sulfate decahydrate (10 g) was added under ice-cooling, and the mixture was filtered through celite. The filtrate was concentrated under reduced pressure and purified by silica gel column chromatography (ethyl acetate/hexane=25/75→60/40) to give the title compound (1.14 g, yield 90%).

WORKUP

后处理

  1. temperaturecooling
  2. filtrationthe mixture was filtered through celite
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. custompurified by silica gel column chromatography (ethyl acetate/hexane=25/75→60/40)