HRID651310
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-cyano-4′-hydroxybiphenyl (56) (10.10 g, 0.052 mol), 1-bromodecane (14.38 g, 0.065 mol), anhydrous potassium carbonate (37.32 g, 0.27 mol), butanone (300 ml) and a trace of potassium iodide was heated under reflux overnight. The cooled solution was filtered to remove inorganic salts and the solvent was removed in vacuo. The residual oil was distilled (to remove excess bromide) and finally purified by column chromatography (dichloromethane) to yield a colourless, low melting solid.
WORKUP
后处理
- temperatureunder reflux overnight
- filtrationThe cooled solution was filtered
- customto remove inorganic salts
- customthe solvent was removed in vacuo
- distillationThe residual oil was distilled
- custom(to remove excess bromide)
- customfinally purified by column chromatography (dichloromethane)
- customto yield a colourless,