HRID2213716

反应详情

EQUATION

反应方程式

HRID 2213716 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A reaction mixture of 141.8 mg (0.59 mmol) of 4-chlorobenzo[g]quinoline-3-carbonitrile, 111.1 mg (0.60 mmol) of 4-phenoxyaniline and 57.8 mg (0.50 mmol) of pyridine hydrochloride in 8 ml of 2-ethoxyethanol is heated at 110–120° C. for 1 hour. After cooling, the mixture is diluted with water and made basic by addition of 125.0 mg (1.18 mmol) of sodium carbonate. The precipitate is collected by filtration and washed with water. Drying in vacuo yields the crude product. The crude product is purified by chromatography, eluting with a methylene chloride/methanol gradient from 100:0 to 86:14, to provide 167.8 mg (73.4%) of the pure product as a yellow solid, mp 250–251° C.

WORKUP

后处理

  1. temperatureis heated at 110–120° C. for 1 hour
  2. temperatureAfter cooling
  3. filtrationThe precipitate is collected by filtration
  4. washwashed with water
  5. customDrying in vacuo
  6. customyields the crude product
  7. customThe crude product is purified by chromatography
  8. washeluting with a methylene chloride/methanol gradient from 100:0 to 86:14