反应详情

Add N-(4oxo-cyclohexyl)-isobutyramide (933 mg, 5.09 mmol) to a suspension of (2,2-difluoro-benzo[1,3]dioxol-5-yl)-hydrazine hydrochloride salt (1.14 g, 5.09 mmol), water (7 mL) and concentrated hydrochloric acid (3 mL). Heat the reaction to 90° C. for 12 h with stirring and cool to ambient temperature. Collect the resultant solid by vacuum filtration, rinse with water and place in a vacuum oven for 5 h to afford the subtitled compound (732 mg, 43%) as a tan solid. 1H NMR (300 MHz, CDCl3): δ 7.96 (br s, 1H), 7.00 (s, 1H), 6.98 (s, 1H), 5.54 (br d, J=7.5 Hz, 1H), 4.40 (br s, 1H), 3.03 (dd, J=15.3, 5.1 Hz, 1H), 2.88-2.71 (m, 2H), 2.51 (dd, J=15.3, 7.0 Hz, 1H), 2.33 (pentet, J=6.9 Hz, 1H), 2.12-1.91 (m, 2H), 1.16 (d, J=6.9 Hz, 6H).

1. temperatureHeat
2. customthe reaction to 90° C. for 12 h
3. customCollect the resultant solid
4. filtrationby vacuum filtration
5. washrinse with water and place in a vacuum oven for 5 h