反应详情

This was prepared using the same procedure as for 5-bromo-3-nitro-4-(4-(1-(pyridin-2-yl)ethyl)piperazin-1-yl)pyridin-2-amine, but here using tert-butyl 4-(1-(pyridin-3-yl)ethyl)piperazine-1-carboxylate (1.1 eq, 0.64 mmol, 186 mg), TFA (2 mL) and CH2Cl2 (2 mL), then 5-bromo-4-chloro-3-nitropyridin-2-amine (147 mg, 0.58 mmol) in iPrOH (3 mL) and DIPEA (1.5 mL). Filtration and washing as previously described gave the product (106 mg, 41% for two steps) as a yellow solid; 1H-NMR (500 MHz, DMSO-d6) 1.33 (d, J=6.7 Hz, 1H, CH3), 3.04 (s, br, 4H, piperazine N(CH2)2), 3.20 (s, br, 4H, piperazine N(CH2)2), 3.59 (q, J=6.8 Hz, 1H, CH), 6.95 (s, br, 2H, NH2), 7.36 (dd, J=7.8, 4.8 Hz, 1H, pyridine H-5), 7.73 (d, br, J=7.8 Hz, 1H, pyridine H-4), 8.14 (s, 1H, bromopyridine H-6), 8.46 (d, br, J=4.7 Hz, 1H, pyridine H-6), 8.52 (s, br, 1H, pyridine H-2);

1. customThis was prepared
2. filtrationFiltration
3. washwashing
4. customas previously described gave the product (106 mg, 41% for two steps) as a yellow solid