反应详情

This was prepared using the same procedure as for 4-(6-bromo-2-(4-(dimethylamino)phenyl)-3H-imidazo[4,5-b]pyridin-7-yl)-N-phenylpiperazine-1-carboxamide, but here using 5-bromo-3-nitro-4-(4-(1-(pyridin-4-yl)ethyl)piperazin-1-yl)pyridin-2-amine (20 mg, 0.049 mmol), DMF (0.15 mL), ethanol (0.85 mL), 1M Na2S2O4 (3 eq, 0.15 mmol, 0.15 mL) and 4-morpholin-4-yl-benzaldehyde (1.1 eq, 0.054 mmol, 10 mg). After 6 h, concentration in vacuo and purification by preparative tlc (CH2Cl2-MeOH, 95:5) gave the product (7 mg, 27%) as an off-white solid; δH (500 MHz, DMSO-d6) 1.36 (d, J=6.4 Hz, 3H, CH3), 2.36 (s, br, 2H, piperazine NCH2), 2.63 (s, br, 2H, piperazine NCH2), 3.30 (hidden by DMSO peak, 4H, morpholine N(CH2)2), 3.58-3.60 (m, 1H, CHCH3), 3.64 (s, br, 4H, piperazine N(CH2)2), 3.76 (t, J=4.6 Hz, 4H, morpholine O(CH2)2), 7.07 (d, J=8.9 Hz, 2H, phenyl H-3 & H-5), 7.39 (d, br, J=6.2 Hz, 2H, pyridine H-3 & H-5), 8.04 (d, J=8.9 Hz, 2H, phenyl H-2 & H-6), 8.16 (s, 1H, imidazo[4,5-b]pyridine H-5), 8.55 (d, br, J=6.0 Hz, 2H, pyridine H-2 & H-6), 13.22 (s, br, 1H, imidazo[4,5-b]pyridine NH);

1. customThis was prepared
2. concentrationconcentration
3. customin vacuo and purification by preparative tlc (CH2Cl2-MeOH, 95:5)