反应详情

LiHMDS (3.0 equivalents) was added to ethyl 3H-imidazo[4,5-b]pyridin-2-ylacetate (1.0 equivalent) in THF at −78° C. After 20 minutes, a solution of 2-amino-6-[(2R,6S)-2,6-dimethylmorpholin-4-yl]benzonitrile (1.1 equivalents) in THF was added. The resulting mixture was allowed to warm to room temperature, stirred for 2 hours, and then it was heated to 60° C. overnight. The mixture was cooled to 0° C. and quenched with an aqueous saturated NH4Cl solution. The aqueous phase was extracted with CH2Cl2 (5 times) and the organic extracts were collected, dried (Na2SO4), and concentrated. The crude product was purified by HPLC. LC/MS m/z 391.2 (MH+), Rt 2.35 minutes.

1. temperatureit was heated to 60° C. overnight
2. temperatureThe mixture was cooled to 0° C.
3. customquenched with an aqueous saturated NH4Cl solution
4. extractionThe aqueous phase was extracted with CH2Cl2 (5 times)
5. customthe organic extracts were collected
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated
8. customThe crude product was purified by HPLC