HRID1837350

反应详情

EQUATION

反应方程式

HRID 1837350 的结构方程式

PROCEDURE

实验过程

A mixture of sodium hydride (500 mg, 12.5 mmol) and 7-fluoro-4-hydroxyquinoline-3-carbonitrile (1.30 g, 6.9 mmol) in 2-methoxyethanol (30 mL) is heated at reflux overnight. Additional sodium hydride (250 mg, 6.25 mmol) is added and the reaction mixture is heated at reflux overnight. Additional sodium hydride (250 mg, 6.25 mmol) is added and the reaction mixture is heated at reflux for 8 hours. The reaction mixture is cooled to room temperature and partitioned between ethyl acetate and saturated sodium bicarbonate. The basic layer is acidified with aqueous HCl and the resultant solid is collected by filtration to provide 1.05 g of 7-(2-methoxyethoxy)-4-oxo-1,4-dihydroquinoline-3-carbonitrile as a white solid, mp>250° C.

WORKUP

后处理

  1. temperatureis heated
  2. temperatureat reflux overnight
  3. temperaturethe reaction mixture is heated
  4. temperatureat reflux overnight
  5. temperaturethe reaction mixture is heated
  6. temperatureat reflux for 8 hours
  7. custompartitioned between ethyl acetate and saturated sodium bicarbonate
  8. filtrationthe resultant solid is collected by filtration