反应详情

温度

75 °C

1H-pyrazole-1-carboximidamide hydrochloride, compound 2-a from Example 2, (22.11 g, 0.15 mol) in EtOH (250 ml) was added sodium methoxide (12.3 g, 0.23 mol) and diethyl ethoxymethylenemalonate, compound 2-b from Example 2, (30 ml, 0.15 mol). The reaction was heated for about 40 min at 75° C. and then cooled to room temperature. The mixture was filtered and the solid was washed with ethanol and ether and dried under vacuum to give compound 3-a (21 g, 60%). 1H NMR (DMSO-d6, 300 MHz): δ 8.50 (m, 2H), 7.70 (s, 1H), 6.47 (m, 1H), 4.13 (m, 2H), 1.24 (m, 3H).

1. temperaturecooled to room temperature
2. filtrationThe mixture was filtered
3. washthe solid was washed with ethanol and ether
4. customdried under vacuum