反应详情

A solution of 3-methyl-4-(2-methylbenzyl)-1H-pyrazol-5-amine (3.005 g, 14.93 mmol) and ethyl 3-oxo-3-(pyridin-4-yl)propanoate (3.17 g, 16.42 mmol) in acetic acid (50 mL) was stirred under reflux for 48 h. After cooled to room temperature, the mixture was concentrated. The residue was diluted with ethyl acetate (30 mL). The resulting precipitate was filtered, washed with ethyl acetate, dried in vacuo to give the titled product (4.02 g, 69%); LC/MS: MS (ES+) m/e 331 (MH+); 1H NMR (300 MHz, DMSO-d6) δ ppm 1.91 (s, 3H), 2.09 (s, 3H), 2.36 (s, 3H), 3.99 (s, 2H), 6.08 (s, 1H), 6.78 (d, J=7.8 Hz, 1H), 7.04-7.21 (m, 3H), 7.77 (d, J=4.8 Hz, 1H), 8.76 (d, J=4.8 Hz, 1H), 11.95 (s, 1H), 12.16 (s, 1H).

1. temperatureunder reflux for 48 h
2. concentrationthe mixture was concentrated
3. additionThe residue was diluted with ethyl acetate (30 mL)
4. filtrationThe resulting precipitate was filtered
5. washwashed with ethyl acetate
6. customdried in vacuo