反应详情

N-{[1,6-Diethyl-4-(tetrahydro-2H-pyran-4-ylamino)-1H-pyrazolo[3,4-b]pyridin-5-yl]methyl}-N′-[(3′-formyl-3-biphenylyl)methyl]-5-methyl-1,3-benzenedicarboxamide (30 mg, 0.046 mmol), 1-methylhexahydro-1H-1,4-diazepine (52 mg, 0.46 mmol, 10 eq) and acetic acid (2.61 μL, 0.046 mmol, 1 eq) were dissolved in DMSO (1.5 mL). The mixture was stirred in VX-2500 Multi-Tube Vortexer for overnight at room temperature. MP-triacetoxyborohydride (137 mg, 0.319 mmol, 7 eq) was then added and the mixture was stirred again in VX-2500 Multi-Tube Vortexer for overnight at room temperature. The reaction mixture was filtered through a polypropylene cartridge (10 mL tube) on Bohdan Miniblock in a reaction tube and concentrated in a Glas-Col evaporator. The reaction mixture was then purified using a Gilson HPLC with a water-acetonitrile with 0.1% TFA buffer. The desired product fractions were combined, filtered through amine cartouche (500 mg) on Bohdan Miniblock and concentrated in a Glas-Col evaporator, giving 9.74 mg (25.4%) of the title compound. LC-MS m/z 757.4 (M+H)+, 1.26 min (ret time).

1. filtrationThe reaction mixture was filtered through a polypropylene cartridge (10 mL tube) on Bohdan Miniblock in a reaction tube
2. concentrationconcentrated in a Glas-Col evaporator
3. customThe reaction mixture was then purified
4. filtrationfiltered through amine cartouche (500 mg) on Bohdan Miniblock
5. concentrationconcentrated in a Glas-Col evaporator