反应详情

温度

80 °C

A mixture of 4-iodo-1H-pyrazole (270 mg, 1.4 mmol), [1-(2,4-dimethoxybenzyl)-3-methyl-5-oxopyrrolidin-3-yl]methyl methanesulfonate (500 mg, 1.4 mmol), cesium carbonate (910 mg, 2.8 mmol), and potassium iodide (10 mg, 0.05 mmol) in DMF (80 mL) was stirred at 80° C. for 12 hours. The mixture was diluted with water and extracted with ethyl acetate. The organic layer was dried over sodium sulfate, filtered, and concentrated under reduced pressure. The residue was purified by chromatography on silica gel (ethyl acetate/petroleum ether) to give 1-(2,4-Dimethoxybenzyl)-4-[(4-iodo-1H-pyrazol-1-yl)methyl]-4-methylpyrrolidin-2-one. MS ESI calc'd. for C18H231 N3O3 [M+H]+ 456. found 456. 1H NMR (400 MHz, MeOD): δ 7.49 (s, 1H), 7.44 (s, 1H), 7.05 (d, J=8 Hz, 1H), 6.54 (d, J=2.4 Hz, 1H), 6.49-6.47 (m, 1H), 4.30 (d, J=4 Hz, 2H), 4.06 (d, J=2 Hz, 2H), 3.78 (s, 6H), 3.33-3.29 (m, 1H), 2.91 (d, J=6.4 Hz, 1H), 2.54 (d, J=16.8 Hz, 1H), 2.17 (d, J=16.8 Hz, 1H), 1.01 (s, 3H).

1. extractionextracted with ethyl acetate
2. dry with materialThe organic layer was dried over sodium sulfate
3. filtrationfiltered
4. concentrationconcentrated under reduced pressure
5. customThe residue was purified by chromatography on silica gel (ethyl acetate/petroleum ether)