HRID544228

反应详情

EQUATION

反应方程式

HRID 544228 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
170 °C

PROCEDURE

实验过程

A mixture of 1-ethyl-6-fluoro-7-chloro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid (1.9 g), piperazine hexahydrate (15 g) and water (15 ml) was heated at 170° C. in a sealed tube for 16 hours. After evaporation of the solvent, the residue was acidified with diluted hydrochloric acid, heated at 100° C., and the hot solution was filtered. The filtrate was evaporated to dryness. The residue was dissolved in 10% sodium hydroxide and neutralized with acetic acid. The precipitate was collected, washed with water, dried, and recrystallized from ethanol to give 1-ethyl-6-fluoro-1,4-dihydro-7-(1-piperazinyl)-4-oxoquinoline-3-carboxylic acid as colorless powder.

WORKUP

后处理

  1. customAfter evaporation of the solvent
  2. temperatureheated at 100° C.
  3. filtrationthe hot solution was filtered
  4. customThe filtrate was evaporated to dryness
  5. dissolutionThe residue was dissolved in 10% sodium hydroxide and neutralized with acetic acid
  6. customThe precipitate was collected
  7. washwashed with water
  8. customdried
  9. customrecrystallized from ethanol