HRID1809706

反应详情

EQUATION

反应方程式

HRID 1809706 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 crude (3-bromo-phenyl)-(2,4-dichloro-pyrimidin-5-yl)-methanone (from Example 37 supra) (1 g, 3.0 mmol) in THF (70 mL), 85% hydrazine (0.45 g, 7.64 mmol) was added dropwise at room temperature. The mixture was stirred for additional 20 minutes at room temperature and then heated at 50° C. for another 20 minutes. The solvent was removed under reduced pressure, and the residue was washed with water (5 mL), petroleum ether (10 mL) and dried to give 3-(3-bromo-phenyl)-6-chloro-1H-pyrazolo[3,4-d]pyrimidine as yellow solid. (Yield 0.848 g, 91.3%).

WORKUP

后处理

  1. temperatureheated at 50° C. for another 20 minutes
  2. customThe solvent was removed under reduced pressure
  3. washthe residue was washed with water (5 mL), petroleum ether (10 mL)
  4. customdried