HRID1266167

反应详情

EQUATION

反应方程式

HRID 1266167 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1-Ethyl-7-fluoro-8-[4-(4-fluorophenyl)piperazin-1-yl]-4-oxo-1,4-dihydrobenzo-[b][1,8]naphthyridine-3-carboxylic acid was prepared under the conditions of Example 2, but from 1.75 g of 8-chloro-1-ethyl-7-fluoro-4-oxo-1,4-dihydrobenzo[b][1,8]naphthyridine-3-carboxylic acid and 3.6 g of 4-(4-fluorophenyl)piperazine in 18 cm3 of pyridine. The solid obtained was taken up in 10 cm3 of water and 1.9 cm3 of 10% acetic acid were added. The suspension was brought to approximately 100° C. The solidified product was filtered off and washed 2 times with 10 cm3 of water and 2 times with 10 cm3 of warm ethanol. After recrystallizing twice from 25 cm3 of dimethylformamide on each occasion, 1.7 g of 1-ethyl-7-fluoro-8-[4-(4-fluorophenyl)piperazin-1-yl]-4-oxo-1,4-dihydrobenzo[b][1,8]naphthyridine-3-carboxylic acid were obtained in the form of a pinkish-beige solid melting at about 311-312° C.

WORKUP

后处理

  1. custom1-Ethyl-7-fluoro-8-[4-(4-fluorophenyl)piperazin-1-yl]-4-oxo-1,4-dihydrobenzo-[b][1,8]naphthyridine-3-carboxylic acid was prepared under the conditions of Example 2
  2. customThe solid obtained
  3. customwas brought to approximately 100° C
  4. filtrationThe solidified product was filtered off
  5. washwashed 2 times with 10 cm3 of water and 2 times with 10 cm3 of warm ethanol
  6. customAfter recrystallizing twice from 25 cm3 of dimethylformamide on each occasion