反应详情

0.5 mol of 4-(trans-4-pentylcyclohexyl)biphenyl, 500 ml of carbon sulfide and 0.5 mol of aluminium chloride are introduced into a three-neck flask fitted with a dry-ice reflux condenser. After the mixture has been cooled to -30°, 0.5 mol of trifluoroacetyl chloride are condensed in. The mixture is then allowed to warm to 0° and stirred at this temperature for 6 hours then at room temperature for 14 hours. The reaction mixture is poured onto a mixture of ice and dilute hydrochloric acid. The organic phase is separated off, and the aqueous phase is extracted by shaking with dichloromethane (2×50 ml). The organic phases are combined, the solvents removed by distillation and the product is recrystallized twice from ethanol.

1. temperaturereflux condenser
2. temperatureAfter the mixture has been cooled to -30°
3. customcondensed in
4. temperatureto warm to 0°
5. waitat room temperature for 14 hours
6. customThe organic phase is separated off
7. extractionthe aqueous phase is extracted
8. stirringby shaking with dichloromethane (2×50 ml)
9. customthe solvents removed by distillation
10. customthe product is recrystallized twice from ethanol