反应详情

BF3Et2O in THF (47-49%) (0.87 mL, 2.46 mmol) was added to a solution of [4-[6-amino-5-(1-isopropyltriazol-4-yl)-3-pyridyl]-2-methyl-phenyl]-morpholino-methanone (200 mg, 0.46 mmol) in THF (10.0 mL) at 0° C. The reaction mixture was stirred for 30 min, NaBH4 (93.5 mg, 2.46 mmol) was added at 0° C., reaction mixture was slowly warmed to RT, stirred for 16 h. Reaction mixture was again cooled to 0° C., added MeOH (5.0 mL) and heated to 70° C. for 2 h. The reaction mixture was diluted with water (50 mL) and extracted with ethyl acetate (2×30 mL). Combined organic layers was dried over Na2SO4 and concentrated under reduced pressure. Crude product was purified by silica (100-200 mesh) column eluted with 2% MeOH in DCM. Product was further purified by Prep.HPLC furnished 30 mg (Yield: 15.5%) of the title compound as a white solid.

1. customreaction mixture
2. stirringstirred for 16 h
3. customReaction mixture
4. temperaturewas again cooled to 0° C.
5. temperatureheated to 70° C. for 2 h
6. extractionextracted with ethyl acetate (2×30 mL)
7. dry with materialCombined organic layers was dried over Na2SO4
8. concentrationconcentrated under reduced pressure
9. customCrude product was purified by silica (100-200 mesh) column
10. washeluted with 2% MeOH in DCM
11. customProduct was further purified by Prep.HPLC