HRID1639751

反应详情

EQUATION

反应方程式

HRID 1639751 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Under nitrogen atmosphere, to a solution of trans-ethyl 2-(2-methyl-2H-indazol-4-yl)cyclopropanecarboxylate (3.89 g, 15.9 mmol) in tetrahydrofuran (100 mL) was added lithium aluminum hydride (0.540 g, 15.9 mmol) at 0° C., and the mixture was stirred for 10 min. To the reaction mixture were added ethyl acetate, water and 10% aqueous sodium hydroxide solution, and the mixture was extracted with ethyl acetate. The extract was washed with 2 N hydrochloric acid and saturated brine, and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by recrystallization (ethyl acetate) to give the title compound (3.00 g, yield 93%).

WORKUP

后处理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe extract was washed with 2 N hydrochloric acid and saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. customThe residue was purified by recrystallization (ethyl acetate)