反应详情

6-[chloro(4-chlorophenyl)(4-methyl-4H-1,2,4-triazol-3-yl)methyl]-4-(3-chlorophenyl)-1-methyl-2(1H)-quinolinone (0.0045 mol) was added at 5° C. to THF (25 ml) under N2 flow. NH3/2-propanol saturated (25 ml) was added dropwise. The mixture was kept for 1 hour, poured out into water and extracted with CH2Cl2. The organic layer was separated, dried (MgSO4), filtered, and the solvent was evaporated till dryness. The residue (2.6 g) was purified by column chromatography over silica gel (eluent: toluene/iPrOH/NH4OH; 50/50/1; 15–40 μm). The pure fractions were collected and the solvent was evaporated. The residue (1.6 g, 73%) was crystallized from CH3CN/DIPE. The precipitate was filtered off and dried. The residue (1.3 g, 59%) was purified by column chromatography over kromasil 10 μm (eluent: CH3OH/H2O; 60/40). The pure fractions were collected and the solvent was evaporated. The residue (1.4 g, 63%) was crystallized from CH3CN/DIPE. The precipitate was filtered off and dried, yielding 1.26 g (57%) of 6-[amino(4-chlorophenyl)(4-methyl-4H-1,2,4-triazol-3-yl)methyl]-4-(3-chlorophenyl)-1-methyl-2(1H)-quinolinone, mp. 210° C.

1. extractionextracted with CH2Cl2
2. customThe organic layer was separated
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. customthe solvent was evaporated till dryness
6. customThe residue (2.6 g) was purified by column chromatography over silica gel (eluent: toluene/iPrOH/NH4OH; 50/50/1; 15–40 μm)
7. customThe pure fractions were collected
8. customthe solvent was evaporated
9. customThe residue (1.6 g, 73%) was crystallized from CH3CN/DIPE
10. filtrationThe precipitate was filtered off
11. customdried
12. customThe residue (1.3 g, 59%) was purified by column chromatography over kromasil 10 μm (eluent: CH3OH/H2O; 60/40)
13. customThe pure fractions were collected
14. customthe solvent was evaporated
15. customThe residue (1.4 g, 63%) was crystallized from CH3CN/DIPE
16. filtrationThe precipitate was filtered off
17. customdried