HRID2213742

反应详情

EQUATION

反应方程式

HRID 2213742 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 722.7 mg (2.70 mmol) of 4,7-dichloro-6-nitro-3-quinolinecarbonitrile, 100.1 mg (2.70 mmol) of 4-phenoxyaniline and 312.1 mg (2.70 mmol) of pyridine hydrochloride in 30 mL of 2-ethoxyethanol is heated at 110–120° C. for 3 hours. After cooling, the mixture is diluted with water, neutralized with an aqueous solution of saturated sodium carbonate, and extracted with ethyl acetate. The separated organic layer is washed with brine and dried over sodium sulfate. Removal of the solvent yields a solid residue which is purified by flash chromatography (elution with 99:1 methylene chloride/methanol), giving 831.0 mg (73.9%) of the product as a deep yellow solid, mp 220–222° C.

WORKUP

后处理

  1. temperatureis heated at 110–120° C. for 3 hours
  2. temperatureAfter cooling
  3. extractionextracted with ethyl acetate
  4. washThe separated organic layer is washed with brine
  5. dry with materialdried over sodium sulfate
  6. customRemoval of the solvent
  7. customyields a solid residue which
  8. customis purified by flash chromatography (elution with 99:1 methylene chloride/methanol)