HRID2291275

反应详情

EQUATION

反应方程式

HRID 2291275 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 5-amino-1-cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid (1.25 g), 2-methylpiperazine (2.0 g), and pyridine (13 ml) was heated at 105°-110° C. for 1 hour with stirring. The reaction mixture was evaporated to dryness under reduced pressure and water was added to the residue. The mixture was extracted with chloroform and the extract was dried. After evaporation of chloroform, ethanol was added to the residue. The resulting crystals were filtered and recrystallized from chloroform-ethanol to give 5-amino-1-cyclopropyl-6,8-difluoro-7-(3-methyl-1-piperazinyl)-1,4-dihydro-4-oxoquinoline-3-carboxylic acid (1.4 g), m.p. 251°-253° C.

WORKUP

后处理

  1. temperaturewas heated at 105°-110° C. for 1 hour
  2. customThe reaction mixture was evaporated to dryness under reduced pressure and water
  3. additionwas added to the residue
  4. extractionThe mixture was extracted with chloroform
  5. customthe extract was dried
  6. customAfter evaporation of chloroform, ethanol
  7. additionwas added to the residue
  8. filtrationThe resulting crystals were filtered
  9. customrecrystallized from chloroform-ethanol