HRID1578259

反应详情

EQUATION

反应方程式

HRID 1578259 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

As described in Example 1, 4.3 g of 6,7-dichloro-1-ethyl-4-oxo-1,4-dihydro-3-quinoline-carboxylic acid and 10.6 g of 1-(β-hydroxyethyl)-piperazine in 45 cm3 of DMSO (dimethylsulphoxide) were heated for 3 hours at 110° C. After evaporation of the solvent under a good vacuum, the viscous residue was taken up in 20 cm3 of isopropanol; the mixture was stirred and heated under reflux for 20 minutes. After standing for one night at 4° C., the solid was filtered off, washed with ethanol and recrystallised from methyl cellosolve (15 cm3). 3.5 g of 6-chloro-1-ethyl-7-[4-(β-hydroxyethyl)-piperazinyl]-4-oxo-1,4-dihydro-quinoline-3-carboxylic acid, m.p. 215° C., were obtained.

WORKUP

后处理

  1. customAfter evaporation of the solvent under a good vacuum
  2. temperatureheated
  3. temperatureunder reflux for 20 minutes
  4. waitAfter standing for one night at 4° C.
  5. filtrationthe solid was filtered off
  6. washwashed with ethanol
  7. customrecrystallised from methyl cellosolve (15 cm3)