反应详情

N2 was bubbled at room temperature to a solution of 4-(3-chlorophenyl)-6-[(4-chlorophenyl)(4-methyl-4H-1,2,4-triazol-3-yl)methyl]-1-methyl-2(1H)-quinolinone (0.00105 mol), obtained in Example B7, in DME (8.5 ml) for 30 minutes. DCM (2 ml) was added. Then 2-methyl, 2-propanol, potassium salt (0.0021 mol) was added portionwise. The mixture was stirred for 1 hour, poured out into water and extracted with DCM. The organic layer was separated, dried (MgSO4), filtered, and the solvent was evaporated till dryness. The residue (0.55 g) was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 100 to 95/5; 10 μm). The pure fractions were collected and the solvent was evaporated. The residue (0.35 g, 64%) was crystallized from CH3CN. The precipitate was filtered off and dried, yielding 0.28 g (51%) of 6-[2-chloro-1-(4-chlorophenyl)-1-(4-methyl-4H-1,2,4-triazol-3-yl)ethyl]-4-(3-chlorophenyl)-1-methyl-2(1H)-quinolinone, mp. 260° C.

1. extractionextracted with DCM
2. customThe organic layer was separated
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. customthe solvent was evaporated till dryness
6. customThe residue (0.55 g) was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 100 to 95/5; 10 μm)
7. customThe pure fractions were collected
8. customthe solvent was evaporated
9. customThe residue (0.35 g, 64%) was crystallized from CH3CN
10. filtrationThe precipitate was filtered off
11. customdried