反应详情

温度

70 °C

To a solution of methyl 5-methyl-1-(4-methylbenzyl)-1H-pyrazole-3-carboxylate (Intermediate A, 16.3 g, 66.7 mmol) in ethanol (500 mL) was added NaOH (1N aq., 133 mL, 133 mmol), and the mixture was heated at 70° C. for 16 h. The organic solvent was evaporated under vacuum and the residue was acidified with HCl (1N aq., 150 mL) until a white solid completely precipitated from solution. The solid was filtered, washed with water (1.5 L), and was dried in a vacuum oven to afford the title compound as a white solid (14.6 g, 95%): 1H NMR (300 MHz, DMSO-d6) 7.0 (d, 2H), 7.08 (d, 2H), 6.56 (s, 1H), 5.35 (s, 2H), 2.30 (s, 3H), 2.27 (s, 3H); ES-MS m/z 231.0 (MH)+, HPLC RT (Method B) 3.12 min.

1. customThe organic solvent was evaporated under vacuum
2. customcompletely precipitated from solution
3. filtrationThe solid was filtered
4. washwashed with water (1.5 L)
5. customwas dried in a vacuum oven