HRID25175

反应详情

EQUATION

反应方程式

HRID 25175 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

3-Ethylaminoazetidine (700 mg), 1-(6-amino-3,5-difluoropyridin-2-yl)-8-bromo-6,7-difluoro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid (1.5 g), N-methyl-pyrrolidine (2.0 g)and dimethylsulfoxide (4.5 g) were combined, and the mixture was heated under stirring at 40° C. for 24 hours. After the mixture was allowed to cool down, isopropyl ether (10 mL) was added, the mixture was stirred, and a clear layer at the top of the mixture was removed. The same procedure was repeated once more, and the residue was concentrated under reduced pressure. Ethanol (5 mL) was added, and the mixture was heated under stirring at 70° C. for 30 minutes. The precipitated solid was collected by filtration. The title compound (1.38 g) was obtained.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureto cool down
  3. stirringthe mixture was stirred
  4. customa clear layer at the top of the mixture was removed
  5. concentrationthe residue was concentrated under reduced pressure
  6. additionEthanol (5 mL) was added
  7. temperaturethe mixture was heated
  8. stirringunder stirring at 70° C. for 30 minutes
  9. filtrationThe precipitated solid was collected by filtration