反应详情

温度

-15 °C

Add Mg turnings (0.25 g, 9.95 mmol) to a solution of 5-Bromoimidazo[1,2-a]pyridine (1.5 g, 7.65 mmol) in tetrahydrofuran (20 ml). Heat the reaction to 60° C. and add bromoethane (1.2 ml, 11.1 mmol). Reflux for another 0.5 hours, cool and cannula dropwise into a solution of diethyl oxalate (5 ml) in tetrahydrofuran (5 ml) at −15° C. Stir at −15° C. for 0.5 hours and at room temperature for 0.5 hours. Quench the reaction by adding pH 7 buffer, extract into ethyl acetate, wash with saturated sodium chloride, dry over magnesium sulfate, and concentrate under reduced pressure. Purification by flash chromatography, eluting with ethyl acetate:hexane:methanol gradient gives the title compound as a light brown oil.

1. temperatureHeat
2. customthe reaction to 60° C.
3. temperatureReflux for another 0.5 hours
4. temperaturecool
5. customat −15° C
6. customQuench
7. customthe reaction
8. additionby adding pH 7 buffer
9. extractionextract into ethyl acetate
10. washwash with saturated sodium chloride
11. dry with materialdry over magnesium sulfate
12. concentrationconcentrate under reduced pressure
13. customPurification by flash chromatography
14. washeluting with ethyl acetate