HRID1094160

反应详情

EQUATION

反应方程式

HRID 1094160 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

2.6 g of 1,1′-carbonyldiimidazole was added to a 30 ml DMF suspension of 4.0 g 7-(cyclohexylamino)-1-cyclopentyl-6-fluoro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid, followed by stirring at 100° C. for 13.5 hours. 10 ml of 28% aqueous ammonia was added thereto under ice-cooling, followed by stirring under ice-cooling for 75 minutes and at room temperature for 5 hours. After evaporation of the solvent under a reduced pressure, ethanol was added, and heating under reflux was carried out. After cooling to room temperature, the insoluble materials were collected by filtration and dried to obtain 3.7 g of 7-(cyclohexylamino)-1-cyclopentyl-6-fluoro-4-oxo-1,4-dihydroquinoline-3-carboxamide.

WORKUP

后处理

  1. temperatureunder ice-cooling
  2. stirringby stirring under ice-
  3. temperaturecooling for 75 minutes and at room temperature for 5 hours
  4. customAfter evaporation of the solvent under a reduced pressure, ethanol
  5. additionwas added
  6. temperatureheating
  7. temperatureunder reflux
  8. temperatureAfter cooling to room temperature
  9. filtrationthe insoluble materials were collected by filtration
  10. customdried