HRID11424

反应详情

EQUATION

反应方程式

HRID 11424 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturethe reaction mixture was heated
  2. temperatureto reflux for 1 h
  3. customThe acetonitrile was removed by evaporation
  4. additionWater (100 ml) was added
  5. customthe mixture was sonicated
  6. customtriturated
  7. filtrationThe resultant off-white solid was then collected by filtration
  8. washwashed with water
  9. customdried under vacuum (0.763 g)