反应详情

温度

80 °C

A mixture of 2-[3-chloro-4-[chloro(4-chlorophenyl)methyl]phenyl]-1,2,4-triazine-3,5(2H,4H)-dione (0.015 mol), 4-hydroxypiperidine (0.02 mol) and sodiumbicarbonate (0.02 mol) in DMF (100 ml) was stirred for 16 hours at 80° C. The mixture was cooled. The solvent was evaporated. The residue was purified by columnchromatography over silica gel (eluent: CH2Cl2/CH3OH 95/5). The desired fractions were collected and the solvent was evaporated. The residue was stirred in DIPE, filtered off and dried, yielding 0.070 g (±)-2-[3-chloro-4-[(4-chlorophenyl)(4-hydroxy-1-piperidinyl)methyl]phenyl]-1,2,4-triazine-3,5(2H,4H)-dione (compound 119).

1. temperatureThe mixture was cooled
2. customThe solvent was evaporated
3. customThe residue was purified by columnchromatography over silica gel (eluent: CH2Cl2/CH3OH 95/5)
4. customThe desired fractions were collected
5. customthe solvent was evaporated
6. stirringThe residue was stirred in DIPE
7. filtrationfiltered off
8. customdried