反应详情

温度

80 °C

Ethyl 2-(5-aminopyridin-2-yl)acetate (1.314 g, 7.29 mmol) dissolved in acetic acid (24.31 ml) and added triethyl orthoacetate (2.69 ml, 14.58 mmol) and sodium azide (0.881 g, 13.55 mmol). The reaction was stirred at 80° C. for 3 hrs. When LC-MS showed reaction was not complete, added more triethyl orthoacetate (2.69 ml, 14.58 mmol) and sodium azide (0.881 g, 13.55 mmol) then continued heating at 80° C. overnight. Evaporated off acetic acid then diluted with ethyl acetate and washed with saturated NaHCO3 solution, brine, then dried over Na2SO4, filtered and concentrated. The crude material was purified by chromatography through an ISCO 40 g Redi-sep column and eluting with 5% MeOH/DCM to yield title compound: LC-MS: M+1=248

1. customreaction
2. temperaturethen continued heating at 80° C. overnight
3. customEvaporated off acetic acid
4. additionthen diluted with ethyl acetate
5. washwashed with saturated NaHCO3 solution, brine
6. dry with materialdried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated
9. customThe crude material was purified by chromatography through an ISCO 40 g Redi-sep column
10. washeluting with 5% MeOH/DCM