反应详情

温度

120 °C

A mixture of 1-(4-methoxybenzyl)-1H-pyrazol-5-amine (3 g, 10 mmol) and (ethoxymethylene)propanedioic acid, diethyl ester (3.8 g, 18 mmol) was heated at 120° C. for 1.5 h, then allowed to cool. After cooling, the mixture was concentrated and the resulting residue was purified with CombiFlash® eluting with 0-30% EtOAc in hexanes to give an intermediate, LCMS (M+H): 374.1. The intermediate was dissolved in diphenyl ether (5 mL). The resulted solution was heated at 240° C. in microwave reactor for 1 h 20 min. After cooling, the solid crashed out was filtered and washed with hexanes to afford 4.0 g (80%) of the sub-title compound. LCMS calc. for C17H18N3O4 (M+H)+: m/z=328.1. Found: 328.1.

1. temperatureto cool
2. temperatureAfter cooling
3. concentrationthe mixture was concentrated
4. customthe resulting residue was purified with CombiFlash®
5. washeluting with 0-30% EtOAc in hexanes
6. customto give an intermediate, LCMS (M+H)
7. temperatureThe resulted solution was heated at 240° C. in microwave reactor for 1 h 20 min
8. temperatureAfter cooling
9. filtrationthe solid crashed out was filtered
10. washwashed with hexanes