反应详情

4-Methylcyclohexanone (170 mg, 1.52 mmol) was mixed with 1-methyl-3,5-dinitro-2-pyridone (300 mg, 1.51 mmol) in 1M methanolic ammonia (30 mL, 30 mmol). The solution was heated at gentle reflux for 3 h. Evaporation of the solvent gave an orange residue which was suspended in CHCl3 and flash chromatographed over silica gel (16 g) eluting with EtOAc/hexane (1:10) to afford a white solid (211 mg, 73% yield): mp 50°-52° C.

1. temperatureThe solution was heated
2. temperatureat gentle reflux for 3 h
3. customEvaporation of the solvent
4. customgave an orange residue which
5. customflash chromatographed over silica gel (16 g)
6. washeluting with EtOAc/hexane (1:10)