HRID358674

反应详情

EQUATION

反应方程式

HRID 358674 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 8-fluoro-1-methyl-4-oxo-1 ,4-dihydro-quinol-3-yl benzoate (10 g), piperidine (3.18 g) and dichloromethane (200 ml) was stirred for 24 hours, a further portion of piperidine (1.7 ml) was added and the stirring continued for a further 24 hours. The solvent was removed by distillation and the residue was triturated with diethyl ether (300 ml). The resultant solid was extracted with aqueous sodium hydroxide (0.1 M, 100 ml) and the extract was neutralised with hydrochloric acid (5M, 2 ml). The resultant precipitate was collected by filtration to give the novel compound 8-fluoro-3-hydroxy-1 -methyl-4-quinolone, m.p. 248°.

WORKUP

后处理

  1. waitthe stirring continued for a further 24 hours
  2. customThe solvent was removed by distillation
  3. customthe residue was triturated with diethyl ether (300 ml)
  4. extractionThe resultant solid was extracted with aqueous sodium hydroxide (0.1 M, 100 ml)
  5. filtrationThe resultant precipitate was collected by filtration