反应详情

温度

60 °C

5-amino-3-(2-hydroxyethoxy)-1H-pyrazole-4-carbonitrile (prepared as described in Middleton, W. J., J. Am. Chem. Soc., 1958, 80, 2829/3.5 g, 20.8 mmol) and dimethylformamide dimethylacetal (4.15 ml, 31.3 mmol) were dissolved in acetonitrile (30 ml) and the mixture was stirred at 60° C. for 1 hour. The solvent was then removed under vacuum and the residue triturated in diethyl ether to provide a white solid, which was filtered and dried under vacuum to give N′-[4-cyano-3-(2-hydroxyethoxy)-1H-pyrazol-5-yl]-N,N-dimethylimidoformamide (4.45 g, 96%); NMR Spectrum: 2.95 (s, 3H), 3.06 (s, 3H), 3.67 (t, 2H), 4.12 (t, 2H) 8.09 (s, 1H); Mass Spectrum: 238 (MH+).

1. customThe solvent was then removed under vacuum
2. customthe residue triturated in diethyl ether
3. customto provide a white solid, which
4. filtrationwas filtered
5. customdried under vacuum