تفاعل #11520

معادلة التفاعل

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

المذيبات

acetonitrile

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe reaction mixture was heated
2. 2
   درجة الحرارةto reflux for 1 h
3. 3
   أخرىThe acetonitrile was removed by evaporation
4. 4
   workup.ADDITIONWater (100 ml) was added
5. 5
   أخرىthe mixture was sonicated
6. 6
   أخرىtriturated
7. 7
   ترشيحThe resultant off-white solid was then collected by filtration
8. 8
   غسيلwashed with water
9. 9
   أخرىdried under vacuum (0.763 g)

الإجراء التجريبي

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).

المصدر