HRID1936333

反应详情

EQUATION

反应方程式

HRID 1936333 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

First, 80 ml of ethanol containing 7.18 g of 4-benzyloxyphenylboronic acid obtained from the synthesis (10-b) above dissolved therein, 50 ml of benzene containing 5.00 g of 1-bromo-4-cyclohexylbenzene dissolved therein, 21.0 ml of a sodium carbonate aqueous solution with a concentration of 2 mol/l, and 0.24 g of tetrakis(triphenylphosphine)palladium(0) were put in an argon-replaced 200 ml flask, and stirred under reflux for eight hours. After the reaction, water and toluene were added to the reaction solution for extraction. The resultant toluene layer was washed with a saturated brine and dried with sodium sulfate. The solvent was then distilled off. The residue was purified by silica gel column chromatography (eluent:toluene/hexane=1/4), to obtain 5.04 g (Y: 70.1%) of 4-benzyloxy-4′-cyclohexylbiphenyl. The purity of the resultant compound was 98.3% as measured by GC.

WORKUP

后处理

  1. dissolutionabove dissolved
  2. temperatureunder reflux for eight hours
  3. additionwere added to the reaction solution for extraction
  4. washThe resultant toluene layer was washed with a saturated brine
  5. dry with materialdried with sodium sulfate
  6. distillationThe solvent was then distilled off
  7. customThe residue was purified by silica gel column chromatography (eluent:toluene/hexane=1/4)