HRID1982160
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureunder reflux in an argon atmosphere for ninety minutes
- dissolutionDuring this time the starting material gradually dissolved
- customto precipitate from solution
- temperatureThe mixture was cooled to -10°
- filtrationthe solids were collected by filtration
- washwere washed in turn with cold acetonitrile and ether