反应详情

To a solution of ethyl piperidine-2-carboxylate hydrochloride (0.5 g, 2.58 mmol) in DMF (15 mL) was added potassium carbonate (1.77 g, 12.89 mmol) at rt. The mixture was stirred at rt for 10 min followed by addition of 5-bromo-2-chloropyrimidine (0.5 g, 2.58 mmol). The reaction was heated up to 80° C. for 3 h. After reaction completion (by TLC), the mixture was poured onto 100 mL ice-cold water and extracted with EtOAc (3×100 mL). The combined organic layer was washed with brine, dried over anhydrous Na2SO4 and evaporated under reduced pressure. The crude residue was purified over 100-200 M silica-gel by using 1.50% EtOAc: hexane to obtain the desired product as an off white solid (0.37 g, 46% yield). MS: 314.08 [M+H]+.

1. temperatureThe reaction was heated up to 80° C. for 3 h
2. customAfter reaction completion (by TLC)
3. extractionextracted with EtOAc (3×100 mL)
4. washThe combined organic layer was washed with brine
5. dry with materialdried over anhydrous Na2SO4
6. customevaporated under reduced pressure
7. customThe crude residue was purified over 100-200 M silica-gel