反应详情

First, 100 ml of ethanol containing 11.89 g of 4-(trans-4-pentylcyclohexyl)phenylboronic acid dissolved therein, 100 ml of benzene containing 10.0 g of 1-bromo-2-fluoro-4-iodobenzene dissolved therein, 33.2 ml of a sodium carbonate aqueous solution with a concentration of 2.0 mol/l, and 0.96 g of tetrakis(triphenylphosphine)palladium(0) were put in an argon-replaced 500 ml flask, and stirred under reflux for 16 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) and recrystallized from acetone, to obtain 11.6 g (Y: 86.8%) of 4-bromo-3-fluoro-4′-(trans-4-pentylcyclohexyl)biphenyl. The purity of the resultant compound was 100.0% as measured by GC.

1. temperatureunder reflux for 16 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)
7. customrecrystallized from acetone