Реакция #11520

Уравнение реакции

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

Растворители

acetonitrile

Условия реакции

Обработка

1. 1
   Температураthe reaction mixture was heated
2. 2
   Температураto reflux for 1 h
3. 3
   ДругоеThe acetonitrile was removed by evaporation
4. 4
   workup.ADDITIONWater (100 ml) was added
5. 5
   Другоеthe mixture was sonicated
6. 6
   Другоеtriturated
7. 7
   ФильтрацияThe resultant off-white solid was then collected by filtration
8. 8
   Промывкаwashed with water
9. 9
   Другоеdried under vacuum (0.763 g)

Методика

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).

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