HRID11424
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
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).
WORKUP
后处理
- temperaturethe reaction mixture was heated
- temperatureto reflux for 1 h
- customThe acetonitrile was removed by evaporation
- additionWater (100 ml) was added
- customthe mixture was sonicated
- customtriturated
- filtrationThe resultant off-white solid was then collected by filtration
- washwashed with water
- customdried under vacuum (0.763 g)