反应详情

1-Amino-2-(2-fluorobenzoyl)pyrrole (41 g, 0.20 mol) and sodium bicarbonate (39 g, 0.46 mol) were combined in 400 ml of dichloromethane. To this stirred slurry was added ethyl chloroformate (24 g, 0.22 mol) over 3 minutes and the reaction mixture was refluxed for 5 hours, whereupon it was quenched with 200 ml of H2O and the organic layer separated. The organic extract was washed with H2O and brine, dried (MgSO4), filtered, and evaporated to an oil which crystallized upon trituration with hexane. Filtration yielded 50.8 g (92%) of crystals, m.p. 78°-80°.

1. temperaturethe reaction mixture was refluxed for 5 hours, whereupon it
2. customwas quenched with 200 ml of H2O
3. customthe organic layer separated
4. extractionThe organic extract
5. washwas washed with H2O and brine
6. dry with materialdried (MgSO4)
7. filtrationfiltered
8. customevaporated to an oil which
9. customcrystallized upon trituration with hexane
10. filtrationFiltration