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 1M 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 1M 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