HRID873347

反应详情

EQUATION

反应方程式

HRID 873347 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
160 °C

PROCEDURE

实验过程

4-(2-(4-Aminophenyl)-1H-benzo[d]imidazol-6-yl)benzene-1,2-diamine (200 mg, 0.64 mmol) and formic acid (0.24 mL, 6.35 mmol) were dissolved in H2O (2 mL) and the mixture heated to 160° C. for 20 min under microwave irradiation. On cooling, a precipitate formed, which was filtered off and washed with water. The filtrate was basified with K2CO3 and stirred for 30 min by which time a precipitate had formed. The mixture was filtered and the precipitate washed with water and dried under suction. The crude product was purified by column chromatography (EtOAc to 85:15 EtOAc-MeOH) to afford the product as a white solid (12 mg, 6%).

WORKUP

后处理

  1. temperatureOn cooling
  2. customa precipitate formed
  3. filtrationwhich was filtered off
  4. washwashed with water
  5. customhad formed
  6. filtrationThe mixture was filtered
  7. washthe precipitate washed with water
  8. customdried under suction
  9. customThe crude product was purified by column chromatography (EtOAc to 85:15 EtOAc-MeOH)