反应详情

A mixture of benzoyl acetonitrile (2.0 g, 13.778 mmol) and methyl hydrazine (0.698, 15.156 mmol) in methanol (10 mL) was irradiated under microwave conditions at 110° C. for 90 min. The reaction mixture was cooled to rt and poured into rapidly stirred ice cold water. The obtained solid was collected by filtration, dried under vacuum and triturated with a mixture of pentane-hexane (˜10 mL) to yield a white solid (1.7 g, 71%). [1H-NMR (CDCl3, 300 MHz) δ 7.82-7.65 (m, 2H), 7.45-7.20 (m, 3H), 5.90 (s, 1H), 3.75 (s, 3H), 3.55 (s, 2H); LCMS RtA=0.824 min; [M+H]+=174.1]

1. customwas irradiated under microwave conditions at 110° C. for 90 min
2. additionpoured into rapidly stirred ice cold water
3. filtrationThe obtained solid was collected by filtration
4. customdried under vacuum
5. customtriturated with a mixture of pentane-hexane (˜10 mL)