HRID647512

反应详情

EQUATION

反应方程式

HRID 647512 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.042 mole of 2-chloro-6-methylpyridine, 0.056 mole of anhydrous potassium carbonate and 0.052 mole of 4-acetamidopyridine in 75 ml of sulfolane are heated to 150° C. with stirring for 24 hours, then the sulfolane is concentrated up to 1.5 of its volume, the mixture is poured into 100 ml of water and extraction is effected four times with 150 ml of diethyl ether. The organic phase is washed with water, it is dried over anhydrous sodium sulfate, concentrated to dryness and the residue is crystallised in 40 m of ethyl acetate. Thus, the 4-acetamido-1-(6-methyl-2-pyridyl)piperidine is obtained; m.p. 145° to 147° C.

WORKUP

后处理

  1. concentrationthe sulfolane is concentrated up to 1.5 of its volume
  2. additionthe mixture is poured into 100 ml of water and extraction
  3. washThe organic phase is washed with water, it
  4. dry with materialis dried over anhydrous sodium sulfate
  5. concentrationconcentrated to dryness
  6. customthe residue is crystallised in 40 m of ethyl acetate