反应详情

温度

75 °C

To a solution of (R)-(1-(5,6-diaminopyridin-2-yl)piperidin-3-yl)(pyrrolidin-1-yl)methanone dihydrochloride (32 mg, 0.088 mmol) in ethanol (0.5 mL) was added triethylamine (50 μL, 1.42 mmol) and acetic acid (82 μL, 1.42 mmol). Then a solution of ethyl 1-(2-methoxyphenyl)cyclopropanecarbimidate hydrochloride (50 mg, 0.09 mmol) in ethanol (0.3 mL) was added and the reaction mixture was heated to 75° C. for 18 h. The solvent was removed under reduced pressure and the residue was partitioned between ethyl acetate and a saturated aqueous solution of sodium bicarbonate. The organic layer was washed with water, dried over sodium sulfate, filtered and concentrated under reduced pressure. The crude material was purified via HPLC to afford the title compound. MS (ESI+) (M+H) 446.1; HPLC retention time: 2.299 min (Method A).

1. customThe solvent was removed under reduced pressure
2. customthe residue was partitioned between ethyl acetate
3. washThe organic layer was washed with water
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe crude material was purified via HPLC