HRID980849
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureto reflux for 6 h
- temperaturethe mixture is cooled
- concentrationconcentrated
- dissolutionThe residue is dissolved in water
- additionammonia is added
- temperaturewith cooling
- filtrationThe precipitated 2-aminobenzimidazole derivative is filtered off with suction
- washwashed with water
- customdried
- customrecrystallized from ethyl acetate and diisopropyl ether, with the addition of active charcoal