反应详情

A stirred solution of 2,3,4,6-tetrafluoroaniline (50 g, 0.30 mole) in benzene (236.6 g, 3.03 mole) was heated under reflux. During a 45 minute period, t-butyl nitrite (46.8 g, 0.455 mole) was added to the reaction mixture. After complete addition the mixture was heated at reflux for 23/4 hours. n-Heptane (1 l) was added, and the solvent was distilled from the reaction flask until a head temperature of 101° was reached. The pot residue was cooled and subjected to column chromatography on silica gel, elution first with n-heptane, then toluene, to give 2,3,4,6-tetrafluoro-[1,1'-biphenyl] (mp, 89°-90°).

1. temperatureunder reflux
2. additionAfter complete addition the mixture
3. temperaturewas heated
4. temperatureat reflux for 23/4 hours
5. distillationthe solvent was distilled from the reaction flask until a head temperature of 101°
6. temperatureThe pot residue was cooled
7. washsubjected to column chromatography on silica gel, elution first with n-heptane