HRID647510

反应详情

EQUATION

反应方程式

HRID 647510 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A mixture of 0.116 moles of 2-chloro-6-phenoxypyridine, 21.5 g of anhydrous potassium carbonate, 0.151 moles of 4-acetamidopyridine and 0.118 mole of copper in powder form in 100 ml of sulfolane is heated to 150° C. with stirring for 40 hours. The sulfolane is distilled, the residue is taken up with water, the suspension is treated with water and it is extracted with methylene chloride. The organic phase is washed with water, dried and concentrated to dryness. By crystallisation of the residue in diisopropylic ether, 4-acetamido-2-(6-phenoxy-2-pyridyl)piperidine is obtained; m.p. 104° to 106° C.

WORKUP

后处理

  1. distillationThe sulfolane is distilled
  2. additionthe suspension is treated with water and it
  3. extractionis extracted with methylene chloride
  4. washThe organic phase is washed with water
  5. customdried
  6. concentrationconcentrated to dryness
  7. customBy crystallisation of the residue in diisopropylic ether