反应详情

In a 500-ml egg plant-type flask, POCl3 (44.46 mL, 0.48 mol) was dropwise added to a DMF (37 mL, 0.48 mol) solution of 1-cyclopropyl-1H-pyrrole (46.46 g, 0.43 mol) with cooling with ice, and then stirred overnight at room temperature. The reaction mixture was poured into 5 N sodium hydroxide solution (336 mL) with cooling with ice, and the reaction solution was made basic with 5 N sodium hydroxide solution added thereto. The mixture solution was extracted with dichloromethane, dried with sodium sulfate, filtered, concentrated, and purified through silica gel column chromatography (Biotage [SiO2, 75+M]) with a hexane/ethyl acetate developer system to obtain the title compound as a colorless oil.

1. temperaturewith cooling with ice
2. temperaturewith cooling with ice
3. additionadded
4. extractionThe mixture solution was extracted with dichloromethane
5. dry with materialdried with sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated
8. custompurified through silica gel column chromatography (Biotage [SiO2, 75+M]) with a hexane/ethyl acetate developer system