HRID980849

反应详情

EQUATION

反应方程式

HRID 980849 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

14.1 g of 1,2-diamino-4-(4-fluorophenylsulfonyloxy)benzene (see Example 1) and 5.8 g of cyanogen bromide in 150 ml of methanol are heated to reflux for 6 h, then the mixture is cooled and concentrated. The residue is dissolved in water, and ammonia is added with cooling. The precipitated 2-aminobenzimidazole derivative is filtered off with suction, washed with water, dried and recrystallized from ethyl acetate and diisopropyl ether, with the addition of active charcoal; melting point 192° C.

WORKUP

后处理

  1. temperatureto reflux for 6 h
  2. temperaturethe mixture is cooled
  3. concentrationconcentrated
  4. dissolutionThe residue is dissolved in water
  5. additionammonia is added
  6. temperaturewith cooling
  7. filtrationThe precipitated 2-aminobenzimidazole derivative is filtered off with suction
  8. washwashed with water
  9. customdried
  10. customrecrystallized from ethyl acetate and diisopropyl ether, with the addition of active charcoal