HRID968780
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
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
A mixture of 6-(Formylamino)-7-methyl-1H-benzimidazole-4-carbonitrile (9) (4.8 kg), water (46 L) and concentrated hydrochloric acid (17.8 kg) is agitated at about 80° C. for about 1½ hours. After the mixture is cooled to about 25° C., a solution of 50% aqueous sodium hydroxide (17.1 kg) and water (64 L) is added. The mixture is cooled to about 25° C. over about 15 minutes. The mixture is then filtered and the product is washed with water (50 L). The product is then dried in a vacuum tray dryer at 45-50° C. and ˜40 torr until dry to obtain 6-Amino-7-methyl-1H-benzimidazole -4-carbonitrile (10) (3.8 kg, 94% yield).
WORKUP
后处理
- temperatureAfter the mixture is cooled to about 25° C.
- temperatureThe mixture is cooled to about 25° C. over about 15 minutes
- filtrationThe mixture is then filtered
- washthe product is washed with water (50 L)
- customThe product is then dried in a vacuum tray dryer at 45-50° C.
- custom˜40 torr until dry