反应详情

To a chilled (0° C.) solution of 2.64 g of methyl 6-aminopyridine-3-carboxylate and 5.5 ml of diisopropylethylamine in 30 ml of dichloromethane under argon is added 6.8 g of 2-biphenylcarbonyl chloride in 10 ml of dichloromethane. The mixture is stirred at room temperature 2 days and then diluted with 120 ml of dichloromethane and 50 ml of water. The organic layer is separated, washed with 50 ml each of 1 M NaHCO3 and brine and dried (Na2SO4). The solution is filtered through a thin pad of hydrous magnesium silicate and the filtrate concentrated under vacuum to give a solid. Crystallization from ethyl acetate gives 6.2 g of white crystals, m.p. 180°-188° C.

1. customThe organic layer is separated
2. washwashed with 50 ml each of 1 M NaHCO3 and brine
3. dry with materialdried (Na2SO4)
4. filtrationThe solution is filtered through a thin pad of hydrous magnesium silicate
5. concentrationthe filtrate concentrated under vacuum
6. customto give a solid
7. customCrystallization from ethyl acetate