反应详情

A mixture of 4.0 g (0.015 mole) of 2,3-bis(4-fluorophenyl)-1-methyl-1H-pyrrole and 3.7 g (0.017 mole) of hexafluoroacetone trihydrate in 75 ml toluene was heated at reflux overnight. Another 3.7 g of hexafluoroacetone trihydrate was added and the mixture was heated at reflux overnight again. An additional 2.0 g of hexafluoroacetone trihydrate was added and the mixture was heated at reflux another eight hours. The mixture was washed twice with water, then the organic layer was dried and concentrated. The crude product was purified by chromatography on silica gel, eluting with hexane/toluene mixtures to give, after recrystallization from hexane, 4.8 g of product, m.p. 130°-131°.

1. temperaturewas heated
2. temperatureat reflux overnight
3. temperaturethe mixture was heated
4. temperatureat reflux overnight again
5. temperaturethe mixture was heated
6. temperatureat reflux another eight hours
7. washThe mixture was washed twice with water
8. customthe organic layer was dried
9. concentrationconcentrated
10. customThe crude product was purified by chromatography on silica gel
11. washeluting with hexane/toluene
12. customto give
13. customafter recrystallization from hexane, 4.8 g of product, m.p. 130°-131°