反应详情

The crude N-(3-Ethyl-1-((6-methylpyridin-2-yl)methyl)-1H-indazol-4-yl)-7-(2-oxoethyl)imidazo[1,2-a]pyridine-3-carboxamide (112 mg, 0.248 mmol), and N-methylpiperazine (25 mg, 0.25 mmol) were dissolved in DCM (5 mL), and treated with 10 equivalents of sodium triacetoxyborohydride, followed by 2 drops of glacial acetic acid. The reaction mixture was stirred at ambient temperature for 48 hours. The reaction mixture was concentrated, and resuspended in saturated aqueous sodium carbonate. The mixture was extracted with DCM and EtOAc, the combined organic layers were dried over anhydrous sodium sulfate, then filtered and concentrated. Purification of the crude material by preparative thin-layer chromatography on silica with 7N NH3-MeOH/MeOH/DCM, 2/8/98 as eluent afforded 83.5 mg of a foamy, white solid. MS (ES+APCI) m/z=537 (M+H) detected.

1. concentrationThe reaction mixture was concentrated
2. extractionThe mixture was extracted with DCM and EtOAc
3. dry with materialthe combined organic layers were dried over anhydrous sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated
6. customPurification of the crude material by preparative thin-layer chromatography on silica with 7N NH3-MeOH/MeOH/DCM, 2/8/98 as eluent
7. customafforded 83.5 mg of a foamy, white solid