反应详情

温度

150 °C

A mixture of tert-butyl 4-(hydrazinocarbonyl)piperidine-1-carboxylate (1.0 g), 4-chlorobenzonitrile (1.7 g), potassium carbonate (0.28 g), and butanol (8.0 mL) was heated at 150° C. for 2 hours using a microwave device. After leaving to be cooled, the solvent was evaporated under reduced pressure, and the residue was azeotroped with toluene. The residue was purified by silica gel column chromatography (chloroform/methanol=100/0 to 90/10). To the purified product was added diisopropyl ether, and the resulting solid was collected by filtration and dried under reduced pressure to obtain tert-butyl 4-[3-(4-chlorophenyl)-1H-1,2,4-triazol-5-yl]piperidine-1-carboxylate (0.62 g).

1. customAfter leaving
2. temperatureto be cooled
3. customthe solvent was evaporated under reduced pressure
4. customthe residue was azeotroped with toluene
5. customThe residue was purified by silica gel column chromatography (chloroform/methanol=100/0 to 90/10)
6. additionTo the purified product was added diisopropyl ether
7. filtrationthe resulting solid was collected by filtration
8. customdried under reduced pressure