반응 #11520

반응 방정식

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

용매

acetonitrile

반응 조건

후처리

1. 1
   온도the reaction mixture was heated
2. 2
   온도to reflux for 1 h
3. 3
   기타The acetonitrile was removed by evaporation
4. 4
   workup.ADDITIONWater (100 ml) was added
5. 5
   기타the mixture was sonicated
6. 6
   기타triturated
7. 7
   여과The resultant off-white solid was then collected by filtration
8. 8
   세척washed with water
9. 9
   기타dried under vacuum (0.763 g)

실험 절차

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).

출처