HRID4568

反应详情

EQUATION

反应方程式

HRID 4568 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1.5 g (0.005 mol) of ethyl 6-fluoro-7-(pyrrol-1-yl)-1-formylamino-4-oxo-1,4-dihydroquinoline-3-carboxylate and 1.3 g (0.01 mol) of potassium carbonate in 10 ml of dimethylformamide is stirred for 3 hours at room temperature, 2.35 g (0.015 mol) of ethyl iodide are then added and the mixture is kept for 4 hours at room temperature. It is poured into a water/ice mixture, the precipitate obtained is filtered off, washed with water and extracted with chloroform, the extract is washed with water, the organic layer is dried, the solvent is evaporated off and the residue is recrystallized from an ethanol/water mixture (1:1) to give 0.7 g of a solid melting at 192°-194° C.

WORKUP

后处理

  1. waitthe mixture is kept for 4 hours at room temperature
  2. customthe precipitate obtained
  3. filtrationis filtered off
  4. washwashed with water
  5. extractionextracted with chloroform
  6. washthe extract is washed with water
  7. customthe organic layer is dried
  8. customthe solvent is evaporated off
  9. customthe residue is recrystallized from an ethanol/water mixture (1:1)