HRID369287

反应详情

EQUATION

反应方程式

HRID 369287 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

Pyridine (500 mg) and a 40% aqueous solution (300 mg) of methylamine were added to 1-(5-amino-2,4-difluorophenyl)-7-fluoro-6-methyl-8-nitro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid (70 mg), and the mixture was heated and stirred overnight at 40° C. Dimethyl sulfoxide (10 drops) was added to the reaction mixture, followed by stirring at 40° C. for 5 hours. The solvent and the like were distilled off under reduced pressure, and ethanol (0.5 ml) was added to the residue. Solids deposited were collected by filtration aid washed with ethanol and diethyl ether to obtain the title compound (53 mg) as a yellow powder.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. stirringby stirring at 40° C. for 5 hours
  3. distillationThe solvent and the like were distilled off under reduced pressure, and ethanol (0.5 ml)
  4. additionwas added to the residue
  5. filtrationSolids deposited were collected by filtration aid
  6. washwashed with ethanol and diethyl ether