反应详情

N-Cyclopropyl-4′-[(2-ethanimidoylhydrazino)carbonyl]-6-methyl-1,1′-biphenyl-3-carboxamide (intermediate 46) (80 mg) in xylene (15 ml) was heated at 190° C. under Dean-Stark conditions for 4 hours. The xylene was decanted from the precipitated solid and the solid washed with cyclohexane. The solid was applied to a bond-elut (silica) and eluted with an ethyl acetate/cyclohexane gradient to give, after evaporation of the solvents under vacuum, N-cyclopropyl-6-methyl-4′-(5-methyl-1,3,4-triazol-2-yl)-1,1′-biphenyl-3-carboxamide.

1. customThe xylene was decanted from the precipitated solid
2. washthe solid washed with cyclohexane
3. washeluted with an ethyl acetate/cyclohexane gradient
4. customto give
5. customafter evaporation of the solvents under vacuum, N-cyclopropyl-6-methyl-4′-(5-methyl-1,3,4-triazol-2-yl)-1,1′-biphenyl-3-carboxamide