反应详情

3-(Boc-methylamino)azetidine (2.74 mmol, 1.0 eq) and 4-chloro-2-methylpyridine HCl (8.21 mmol, 3.0 eq) were dissolved in 2-propanol (5 ml) and DI PEA (13.69 mmol. 5.0 eq) and refluxed for 24 hours. After monitoring by TLC, the reaction solution was diluted with ethyl acetate and sat. sodium hydrogen carbonate solution, and the phases were separated. The aqueous phase was washed with ethyl acetate. The combined organic phases were washed 1× with sat. NaCl solution, dried over magnesium sulfate, concentrated under reduced pressure. The crude product was purified by column chromatography (silica gel, ethyl acetate:ethanol 10:1+ammonia solution). Yield: 51%

1. temperatureDI PEA (13.69 mmol. 5.0 eq) and refluxed for 24 hours
2. customthe phases were separated
3. washThe aqueous phase was washed with ethyl acetate
4. washThe combined organic phases were washed 1× with sat. NaCl solution
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated under reduced pressure
7. customThe crude product was purified by column chromatography (silica gel, ethyl acetate:ethanol 10:1+ammonia solution)