Potassium Carbonate → 6-Bromo-2,3-dimethylimidazo(1,2-a)pyridine

13.53 mL (130.06 mmol) of 3-bromobutan-2-one are added to a mixture, stirred at 20° C., of 5 g (28.90 mmol) of 2-amino-5-bromopyridine and 4.85 g (57.80 mmol) of sodium hydrogen carbonate in 100 mL of ethanol. The mixture is refluxed for 12 hours and then concentrated under reduced pressure. The mixture obtained is taken up in 100 mL of water. The pH of the solution is basified by successive additions of potassium carbonate. The mixture is then extracted with 3×50 mL of ethyl acetate. The combined organic phases are washed with water (50 mL), dried over sodium sulfate and then concentrated under reduced pressure. An oil is obtained, which is purified by chromatography on a column of silica, eluting with a mixture of dichloromethane and methanol. 1.1 g of the expected product are thus isolated.

1. temperatureThe mixture is refluxed for 12 hours
2. concentrationconcentrated under reduced pressure
3. customThe mixture obtained
4. extractionThe mixture is then extracted with 3×50 mL of ethyl acetate
5. washThe combined organic phases are washed with water (50 mL)
6. dry with materialdried over sodium sulfate
7. concentrationconcentrated under reduced pressure
8. customAn oil is obtained
9. customwhich is purified by chromatography on a column of silica
10. washeluting with a mixture of dichloromethane and methanol

ORD 기록

ord-45ac94157fe94ece9503285807d874bb

출처 데이터셋

uspto-grants-2013_03

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US08394820B2