HRID1982160

反应详情

EQUATION

反应方程式

HRID 1982160 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-(8-bromodibenz[b,f]oxepin-10-yl)pyridine (2.0 g) in acetonitrile (30 ml) containing methyl iodide (1.1 ml) was stirred under reflux in an argon atmosphere for ninety minutes. During this time the starting material gradually dissolved and a yellow solid began to precipitate from solution. The mixture was cooled to -10° and the solids were collected by filtration and were washed in turn with cold acetonitrile and ether to give 2.7 g of 4-(8-bromo-dibenz[b,f]oxepin-10-yl)-1-methylpyridinium iodide.

WORKUP

后处理

  1. temperatureunder reflux in an argon atmosphere for ninety minutes
  2. dissolutionDuring this time the starting material gradually dissolved
  3. customto precipitate from solution
  4. temperatureThe mixture was cooled to -10°
  5. filtrationthe solids were collected by filtration
  6. washwere washed in turn with cold acetonitrile and ether