HRID1703787

反应详情

EQUATION

反应方程式

HRID 1703787 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionadd 200 ml
  2. temperaturereflux the reaction mixture for 4 hours
  3. concentrationConcentrate the reaction mixture
  4. dissolutiondissolve the resulting solid residue in 2 liters of methylene chloride
  5. washWash the methylene chloride solution with three 500 ml portions of water
  6. dry with materialdry the resulting solution over sodium sulfate
  7. concentrationconcentrate
  8. customtriturate the solid residue with petroleum ether