HRID1073628

反应详情

EQUATION

反应方程式

HRID 1073628 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 1.5 g of (RS)-3-ethoxycarbonyl-7,9-difluoro-1-methyl-8-(3-methyl-1-piperazinyl)-4-oxo-1,4-dihydro-benzo[b][1,8]naphthyridine in 20 cm3 of ethanol and 20 cm3 of N aqueous potassium hydroxide solution is heated at a temperature close to 75° C. for 1 hour and a half. 12 g of a 10% aqueous solution of acetic acid is added to the solution obtained, at this latter temperature. The insoluble matter obtained is drained at about 75° C. and washed 3 times with 30 cm3 of water at about 20° C. After recrystallizing once from 100 cm3 of dimethylformamdide, 0.9 g of (RS)-7,9-difluoro-1-methyl-8-(3-methyl-1-piperazinyl)-4-oxo-1,4-dihydro-benzo[b][1,8]naphthyridine-3-carboxylic acid is obtained in the form of a yellow solid melting at 380°-382° C.

WORKUP

后处理

  1. temperatureis heated at a temperature
  2. customclose to 75° C. for 1 hour
  3. customobtained, at this latter temperature
  4. customThe insoluble matter obtained
  5. customis drained at about 75° C.
  6. washwashed 3 times with 30 cm3 of water at about 20° C
  7. customAfter recrystallizing once from 100 cm3 of dimethylformamdide