HRID4565

反应详情

EQUATION

反应方程式

HRID 4565 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A mixture of 6 g (0.02 mol) of ethyl 6-fluoro-7-(pyrrol-1-yl)-4-hydroxyquinoline-3-carboxylate and 5.6 g (0.04 mol) of potassium carbonate in 80 ml of dimethylformamide is heated for 30 minutes at 60° C. and left to cool, 8.5 g (0.042 mol) of 2,4-dinitrophenylhydroxylamine are added, the mixture is kept for 24 hours at room temperature and poured into 200 ml of a water/ice mixture, and the precipitate formed is filtered off, washed with water, dried in a desiccator and recrystallized from dimethylformamide to give 1.5 g of a solid melting at 276°-279° C.

WORKUP

后处理

  1. waitleft
  2. temperatureto cool
  3. customthe precipitate formed
  4. filtrationis filtered off
  5. washwashed with water
  6. customdried in a desiccator
  7. customrecrystallized from dimethylformamide