反应详情

A mixture of 20.4 g (0.08 mole) of 2,3-bis(4-fluorophenyl)-1H-pyrrole and 19.8 g (0.09 mole) of hexafluoroacetone trihydrate in 300 ml toluene was heated at reflux for 6 hours. Analysis by tlc indicated a small amount of starting material remained so another 1.0 g of hexafluoroacetone trihydrate was added and the mixture was refluxed another 0.5 hour. After stirring at room temperature overnight, the mixture was concentrated by rotary evaporation. The residue was purified by chromatography on 2 pounds of silica gel, eluting with toluene. The chromatographed product was decolorized with charcoal, then recrystallized from hexane to give 21.5 g (63%) of product, m.p. 112°-113°.

1. temperaturewas heated
2. temperatureat reflux for 6 hours
3. additionwas added
4. temperaturethe mixture was refluxed another 0.5 hour
5. concentrationthe mixture was concentrated by rotary evaporation
6. customThe residue was purified by chromatography on 2 pounds of silica gel
7. washeluting with toluene
8. customrecrystallized from hexane