反应 #11520

反应方程式

ammonia

Hydroxybenztriazole

1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride

5-Bromo-3-[(t-butyloxycarbonyl)amino]thiophene-2-carboxylic acid

→

5-Bromo-3-(t-butyloxycarbonyl)aminothiophene-2-carboxamide

溶剂

acetonitrile

反应条件

后处理

1. 1
   温度the reaction mixture was heated
2. 2
   温度to reflux for 1 h
3. 3
   其他The acetonitrile was removed by evaporation
4. 4
   workup.ADDITIONWater (100 ml) was added
5. 5
   其他the mixture was sonicated
6. 6
   其他triturated
7. 7
   过滤The resultant off-white solid was then collected by filtration
8. 8
   洗涤washed with water
9. 9
   其他dried under vacuum (0.763 g)

实验过程

5-Bromo-3-[(t-butyloxycarbonyl)amino]thiophene-2-carboxylic acid (0.80 g) was stirred in acetonitrile (80 ml). Hydroxybenztriazole (1.41 g) and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (2.62 g) were added and stirring continued at room temperature for 10 minutes. Concentrated aqueous ammonia solution (8 ml) was added and the reaction mixture was heated to reflux for 1 h. The acetonitrile was removed by evaporation. Water (100 ml) was added and the mixture was sonicated and triturated. The resultant off-white solid was then collected by filtration, washed with water and dried under vacuum (0.763 g).

来源