反应详情

A mixture of 4.2 g (0.01 mole) of 4,5-bis(4-fluorophenyl)-α,α-di(trifluoromethyl)-1H-pyrrole-2-methanol and 100 ml acetic anhydride was heated at reflux under nitrogen for 3 hours. The mixture was cooled and concentrated under vacuum. The residue was purified by column chromatography on 400 g of silica gel. Eluted with 50/50 hexane/toluene was 4,5-bis(4-fluorophenyl)-2[2,2,2-trifluoro-1-(trifluoromethyl)-ethylidene]-2H-pyrrole, obtained after recrystallization from hexane as a yellow-orange solid, 1.8 g (45%), m.p. 145°-146°. The ir and nmr (proton and fluorine) spectra were consistent with the assigned structure.

1. temperaturewas heated
2. temperatureat reflux under nitrogen for 3 hours
3. temperatureThe mixture was cooled
4. concentrationconcentrated under vacuum
5. customThe residue was purified by column chromatography on 400 g of silica gel
6. washEluted with 50/50 hexane/toluene
7. customobtained
8. customafter recrystallization from hexane as a yellow-orange solid, 1.8 g (45%), m.p. 145°-146°