HRID1703787
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
To a stirred suspension of 238 g of 1-(4'-chloro[1,1']biphenyl-4-yl)ethanol in 2 liters of anhydrous benzene add 200 ml. of thionyl chloride over 40 minutes. With stirring, reflux the reaction mixture for 4 hours. Concentrate the reaction mixture and dissolve the resulting solid residue in 2 liters of methylene chloride. Wash the methylene chloride solution with three 500 ml portions of water, dry the resulting solution over sodium sulfate, concentrate, and triturate the solid residue with petroleum ether to yield 4'-chloro-4-(1-chloroethyl)[1,1']-biphenyl m.p. 100°-102° C.
WORKUP
后处理
- additionadd 200 ml
- temperaturereflux the reaction mixture for 4 hours
- concentrationConcentrate the reaction mixture
- dissolutiondissolve the resulting solid residue in 2 liters of methylene chloride
- washWash the methylene chloride solution with three 500 ml portions of water
- dry with materialdry the resulting solution over sodium sulfate
- concentrationconcentrate
- customtriturate the solid residue with petroleum ether