HRID1936335

反应详情

EQUATION

反应方程式

HRID 1936335 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

First, 100 ml of ethanol containing 4.91 g of 4-(trans-4-pentylcyclohexyl)phenylboronic acid dissolved therein, 100 ml of benzene containing 10.0 g of 2-trifluoromethyl-4-bromoaniline, 41.7 ml of a sodium carbonate aqueous solution with a concentration of 2 mol/l, and 1.20 g of tetrakis(triphenylphosphine)palladium(0) were put in an argon-replaced 300 ml flask, and stirred under reflux for six hours. After the reaction, water and ether were added to the reaction solution for extraction. The resultant ether 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:hexane/toluene=4/1), to obtain 14.82 g (Y: 91.3%) of 4-amino-4′-(trans-4-pentylcyclohexyl)-3-trifluoromethylbiphenyl. The purity of the resultant compound was 99.2% as measured by GC.

WORKUP

后处理

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