反应详情

温度

80 °C

To a solution of 3-methyl-4-{[2-methyl-3-(trifluoromethyl)phenyl]methyl}-1H-pyrazol-5-amine (2.0 g, 7.43 mmol), dimethyl propanedioate (1.03 g, 7.8 mmol) and in methanol (20 mL) stirred under nitrogen at 20° C. was added a solution of sodium methoxide (3.21 g, 14.9 mmol) in methanol (20 mL) dropwise during 15 minutes. The reaction mixture was stirred at 80° C. for overnight. After the reaction mixture was cooled to room temperature, precipitate was collected by filtration, then washed with methanol (5 mL×2). Product was dried under air. The product was then suspended with 1 N HCl (10 mL), stirred for 10 minutes, and filtered off HCl solution. The product was dried and used in next step without further purification. (2.41 g, 96%); LC/MS: MS (ES+) m/e 338 (MH+).

1. temperatureAfter the reaction mixture was cooled to room temperature
2. filtrationprecipitate was collected by filtration
3. washwashed with methanol (5 mL×2)
4. customProduct was dried under air
5. stirringstirred for 10 minutes
6. filtrationfiltered off HCl solution
7. customThe product was dried
8. customused in next step without further purification