反应 #335607

反应方程式

Hydroxylamine O-sulphonic acid

2-aminobenzimidazole

potassium hydroxide

→

1,2-Diaminobenzimidazole

溶剂

water

反应条件

后处理

1. 1
   其他to precipitate
2. 2
   过滤the product collected by filtration
3. 3
   洗涤washed with water
4. 4
   其他dried in air at ambient temperature
5. 5
   workup.WAITOn standing overnight
6. 6
   其他a second crop, 5.8 g was obtained
7. 7
   其他16.55 g, 60%, mp. 252°-254° C., (lit. 255°-259° C.)
8. 8
   其他This was used without further purification (note 1)

实验过程

Hydroxylamine O-sulphonic acid (tech. 23.25 g, 205 mmol) was added to a stirred solution of 2-aminobenzimidazole (25 g, 187.5 mmol) dissolved in water (600 ml) containing potassium hydroxide (24.6 g, 438 mmol) at 23° C. After a few moments a white solid began to precipitate. The mixture was stirred for 30 mins and the product collected by filtration, washed with water and dried in air at ambient temperature, 10.75 g. On standing overnight a second crop, 5.8 g was obtained. The total yield of product was 16.55 g, 60%, mp. 252°-254° C., (lit. 255°-259° C.). Spectroscopic analysis was consistent with the product but indicated a small amount of the starting material was also present. This was used without further purification (note 1).

来源