HRID2304564

反应详情

EQUATION

反应方程式

HRID 2304564 的结构方程式

PROCEDURE

实验过程

A suspension of ethyl 4-methyl-2-oxo-1,2-dihydro-3-quinolinecarboxylate (obtained according to 3.a, 15.2 g, 0.066 mol) in phosphoryl chloride (243 ml) is taken to reflux for 6 hours. The phosphoryl chloride is evaporated under reduced pressure without taking to dryness, and the viscous residue is poured into ice cold water (300 ml). The precipitate obtained in this way is filtered, washed with water to a neutral pH, then washed with ethanol and with diethyl ether in order to produce after drying 8.8 g (53%) of a white solid, m.p. 110° C.

WORKUP

后处理

  1. temperatureto reflux for 6 hours
  2. customThe phosphoryl chloride is evaporated under reduced pressure
  3. additionthe viscous residue is poured into ice cold water (300 ml)
  4. customThe precipitate obtained in this way
  5. filtrationis filtered
  6. washwashed with water to a neutral pH
  7. washwashed with ethanol and with diethyl ether in order
  8. customto produce
  9. dry with materialafter drying 8.8 g (53%) of a white solid, m.p. 110° C.