HRID481292

反应详情

EQUATION

反应方程式

HRID 481292 的结构方程式

PROCEDURE

实验过程

200 ml of ethanol and 100 ml (1.88 mol) of concentrated sulfuric acid were added to 55.5 g of 5-methylpyridine-2-carbonitrile to form a homogeneous solution, followed by heating under reflux for 2 days. The reaction liquid was gradually poured into a saturated aqueous solution of sodium hydrogencarbonate under cooling with ice to neutralize the sulfuric acid, followed by extraction with dichloromethane. The organic layer was washed with a saturated aqueous solution of common salt and dried over anhydrous sodium sulfate. After filtration, the filtrate was concentrated in a reduced pressure to give 78.1 g of a brown oil of the title compound as the crude product.

WORKUP

后处理

  1. customto form a homogeneous solution
  2. temperatureby heating
  3. temperatureunder reflux for 2 days
  4. customThe reaction liquid
  5. temperatureunder cooling with ice
  6. extractionfollowed by extraction with dichloromethane
  7. washThe organic layer was washed with a saturated aqueous solution of common salt
  8. dry with materialdried over anhydrous sodium sulfate
  9. filtrationAfter filtration
  10. concentrationthe filtrate was concentrated in a reduced pressure