HRID271406

反应详情

EQUATION

反应方程式

HRID 271406 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a stirred solution of 4-chloro-6-(4-chlorophenyl)pyrimidine (1.25 g, 5.6 mmol) in THF (10 mL) at room temperature under argon was added H2NNH2 (538 mg, 16.8 mmol). The reaction mixture was heated at 60° C. under argon for 2 h. Analysis by HPLC/MS indicated that the reaction was complete. About three fourths of the solvent was evaporated and Et2O (5 mL) was added to the resulting suspension. After stirring at room temperature for 20 min, solid was collected by filtration and further washed with Et2O (15 mL), then dried under vacuum to obtain 831 mg of the title compound as a white solid. HPLC/MS: retention time=1.88 min, [M+H]30 =221.

WORKUP

后处理

  1. customAbout three fourths of the solvent was evaporated
  2. additionEt2O (5 mL) was added to the resulting suspension
  3. filtrationsolid was collected by filtration
  4. washfurther washed with Et2O (15 mL)
  5. customdried under vacuum