HRID4566

反应详情

EQUATION

反应方程式

HRID 4566 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of 3.15 g (0.01 mol) of ethyl 6-fluoro-7-(pyrrol-1-yl)-1-amino-4-oxo-1,4-dihydroquinoline-3-carboxylate in 25 ml of formic acid is added dropwise to a mixture of 9.5 ml (0.01 mol) of acetic anhydride and 4 ml (0.01 mol) of formic acid, cooled to 0° C., the addition being carried out so as to maintain room temperature ±5° C. The mixture is kept at room temperature for48 hours and poured into a water/ice mixture, and the precipitate formed is filtered off, washed with water and recrystallized from a dimethylformamide/water mixture (1:1) to give a solid melting at 254°-257° C.

WORKUP

后处理

  1. additionthe addition
  2. temperatureto maintain room temperature ±5° C
  3. waitThe mixture is kept at room temperature for48 hours
  4. customthe precipitate formed
  5. filtrationis filtered off
  6. washwashed with water
  7. customrecrystallized from a dimethylformamide/water mixture (1:1)