HRID1981898

反应详情

EQUATION

反应方程式

HRID 1981898 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

8,9-Difluoro-2-methyl-7-nitro-6-oxo-1,2-dihyro-pyrrolo[3,2,1-ij]quinoline-5-carboxylic acid (6 g) is dissolved in dimethylformamide (300 ml) and thereto is added 20% palladium-carbon catalyst (0.5 g), and the mixture is subjected to a catalytic reduction under a pressure of 5 kg/cm2. After the reaction, the cartalyst is filtered off and further dimethylformamide is distilled off, and to the residue is added ethanol. The resulting precipited crystals are separated by filtration and recrystallized from dimethylformamide to give 8,9-difluoro-2-methyl-7-amino-6-oxo-1,2-dihydro-pyrrolo[3,2,1-ij]quinoline-5-carboxylic acid (2.7 g) as yellow cubic crystals. m.p. 270°-274° C. (decomp.)

WORKUP

后处理

  1. customAfter the reaction
  2. filtrationthe cartalyst is filtered off
  3. distillationfurther dimethylformamide is distilled off
  4. additionto the residue is added ethanol
  5. customThe resulting precipited crystals are separated by filtration
  6. customrecrystallized from dimethylformamide