反应详情

N-{[1,6-Diethyl-4-(tetrahydro-2H-pyran-4-ylamino)-1H-pyrazolo[3,4-b]pyridin-5-yl]methyl}-N′-[(6-fluoro-3′-formyl-3-biphenylyl)methyl]-1,3-benzenedicarboxamide (50.0 mg. 0.076 mmol) was diluted in DMSO (1.0 mL) and dispensed into a 1 dram vial containing 2,6-dimethylpiperazine (0.76 mmol), ZnCl2 (0.032 mmol, 4.2 mg), NaB(OAc)3H (0.76 mmol, 180 mg), with fitted magnetic stir bar, for 12 h. Purification was completed via a Gilson HPLC and desired product collected. The product was dissolved in dichloromethane (1 mL) and washed though 2 g of SPE-Amine in a column (EtOAc:MeOH=4:1, 5 mL) to afford 29.9 mg of the title compound (51.6%). LC-MS m/z 762 (M+H)+, 1.38 min (ret time).

1. customwith fitted magnetic stir bar
2. customPurification
3. customcollected
4. dissolutionThe product was dissolved in dichloromethane (1 mL)
5. washwashed though 2 g of SPE-Amine in a column (EtOAc:MeOH=4:1, 5 mL)