反应详情

To a solution of 1-{5-[4-(3,4-dichloro-phenyl)-1H-imidazol-2-yl]-pyridin-2-yl}-piperazine (150 mg, 0.40 mmol) in chloroform (10 ml) was added 4-dimethylaminopyridine (50 mg, 0.44 mmol, 1.1 equiv), followed by furan-2-carbonyl chloride (40 μl, 53 mg, 0.44 mmol, 1.1 equiv). The reaction was stirred for two days at room temperature. The reaction mixture was then diluted with dichloromethane (10 ml) and extracted with an aqueous solution of saturated sodium bicarbonate (2×10 ml), dried over anhydrous magnesium sulfate, filtered, and concentrated in vacuo. Purification of the residue by flash column chromatography (20% ethyl acetate/hexanes grading to 100% ethyl acetate, then 10% methanol/dichloromethane) provided the desired product (110 mg, 59%). MS m/z 468 (M++1).

1. extractionextracted with an aqueous solution of saturated sodium bicarbonate (2×10 ml)
2. dry with materialdried over anhydrous magnesium sulfate
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customPurification of the residue by flash column chromatography (20% ethyl acetate/hexanes grading to 100% ethyl acetate