HRID27042

反应详情

EQUATION

反应方程式

HRID 27042 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

In 200 ml dimethyl sulfoxide (DMSO) was dissolved 25.0 g (0.225 mole) 4-mercaptopyridine. To this solution were added 15.5 g (0.112 mole) anhydrous potassium carbonate and 16.5 g (0.25 mole) propargyl chloride. This mixture was heated at 60° C. for 3 hours. The reaction mixture was then cooled to room temperature and filtered. The filtrate was added to an equal volume of water. This mixture was extracted with ether. After removal of the ether under reduced pressure, there remained 20.0 g crude product. Distillation gave 13.5 g 4-(2-propynylthio)pyridine. Yield 39% theory; b.p. 79°-81° C. (1.0 mm); mp 55°-56° C.

WORKUP

后处理

  1. temperatureThe reaction mixture was then cooled to room temperature
  2. filtrationfiltered
  3. additionThe filtrate was added to an equal volume of water
  4. extractionThis mixture was extracted with ether
  5. customAfter removal of the ether under reduced pressure, there
  6. distillationDistillation