反应详情

5-Amino-2-methyl-2H-pyrazole-3-carboxylic acid methyl ester (644, 1.3 g, 8.0 mmol) was combined with 3-chlorobenzaldehyde (645, 0.95 mL, 8.4 mmol) and acetonitrile (40 mL). Trifluoroacetic acid (3.2 mL, 42.0 mmol) was added followed by triethylsilane (6.7 mL, 42.0 mmol). The reaction was heated to reflux overnight and then concentrated. Ethyl acetate was added and the solution was washed with 1N potassium carbonate. The organic portion was dried over anhydrous sodium sulfate, filtered and concentrated. The compound (646, 0.944 g, 42%) was crystallized from a mixture of ethyl acetate:hexane.

1. temperatureThe reaction was heated
2. temperatureto reflux overnight
3. concentrationconcentrated
4. additionEthyl acetate was added
5. washthe solution was washed with 1N potassium carbonate
6. dry with materialThe organic portion was dried over anhydrous sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated
9. customThe compound (646, 0.944 g, 42%) was crystallized from a mixture of ethyl acetate