HRID1434520

反应详情

EQUATION

反应方程式

HRID 1434520 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.8 g (7.7 mmol) 1-(3-fluoro-4-nitro-phenyl)-1H-pyridin-2-one are dissolved in 360 ml of ethanol, combined with 8.7 g (38.4 mmol) tin(II)chloride-hydrate and refluxed for 45 min. The mixture is cooled and concentrated to dryness. The residue is combined with equal amounts of 1N sodium hydroxide solution and ethyl acetate. The precipitate is filtered off, water is added to the filtrate, the organic phase is separated off and the aqueous phase is extracted twice with ethyl acetate. The combined organic phases are dried over sodium sulphate and evaporated to dryness.

WORKUP

后处理

  1. temperaturerefluxed for 45 min
  2. temperatureThe mixture is cooled
  3. concentrationconcentrated to dryness
  4. filtrationThe precipitate is filtered off
  5. additionwater is added to the filtrate
  6. customthe organic phase is separated off
  7. extractionthe aqueous phase is extracted twice with ethyl acetate
  8. dry with materialThe combined organic phases are dried over sodium sulphate
  9. customevaporated to dryness