反应详情

To a mixture of 0.57 g (0.015 mole) of lithium aluminum hydride in 200 ml ether under nitrogen was added dropwise a solution of 4.03 g (0.01 mole) of 4,5-bis(4-fluorophenyl)-2-[2,2,2-trifluoro-1-(trifluoromethyl)ethylidene]-2H-pyrrole in 50 ml ether. The mixture was stirred at room temperature for 2 hours, then water was added cautiously dropwise. Finally approximately 50 ml of 1 N HCl was added and the ether layer was separated. The aqueous layer was further extracted with ether. The combined ether layers were dried and concentrated under vacuum. The residue was purified by column chromatography on 450 g slica gel, eluting with 75/25 hexane/toluene to give, after recrystallization from hexane, 1.6 g (40%) of product, m.p. 123°-124°, identical by ir and tlc to product obtained by Method A.

1. customthe ether layer was separated
2. extractionThe aqueous layer was further extracted with ether
3. dry with materialThe combined ether layers were dried
4. concentrationconcentrated under vacuum
5. customThe residue was purified by column chromatography on 450 g slica gel
6. washeluting with 75/25 hexane/toluene
7. customto give
8. customafter recrystallization from hexane, 1.6 g (40%) of product, m.p. 123°-124°