HRID968780

反应详情

EQUATION

反应方程式

HRID 968780 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureAfter the mixture is cooled to about 25° C.
  2. temperatureThe mixture is cooled to about 25° C. over about 15 minutes
  3. filtrationThe mixture is then filtered
  4. washthe product is washed with water (50 L)
  5. customThe product is then dried in a vacuum tray dryer at 45-50° C.
  6. custom˜40 torr until dry