反应详情

温度

25 °C

To a solution of 50 mg of 4-{1-[2-(4-Acetyl-3,5-dimethyl-piperazin-1-yl)-pyridin-4-yl]-1H-[1,2,4]triazol-3-ylamino}-benzoic acid (0.11 mMol, 1.0 equiv) in 10 mL of CH2Cl2 and 5 mL of DMF was added 500 μL of Hunig's base followed by 50 mg of DPPA (0.18 mMol, 1.6 equiv). The reaction was stirred for 30 min at 25° C. and then diluted with 10 mL of MeOH and warmed to 80° C. for 12 hr. The reaction was concentrated and purified by flash chromatography (10:1 CH2Cl2:MeOH) to yield 7 mg of 3-(4-{1-[2-(4-Acetyl-3,5-dimethyl-piperazin-1-yl)-pyridin-4-yl]-1H-[1,2,4]triazol-3-ylamino}-phenyl)-1,1-dimethyl-urea (0.015 mMol, 13% yield). 1H NMR (500 MHz, CDCl3) ∂ 8.31 (1H, s), 8.13 (1H, d), 7.40 (2H, d), 7.30 (2H, d), 6.95 (1H, s), 6.82 (1H, d), 6.70 (1H, s), 6.18 (1H, s), 4.15 (2H, m), 3.10 (2H, m), 2.99 (6H, s), 2.90 (2H, m), 2.10 (3H, s), 1.35 (6H, d) ppm. LC/MS: 1.92 min/478.1 (M+1)

1. temperaturewarmed to 80° C. for 12 hr
2. concentrationThe reaction was concentrated
3. custompurified by flash chromatography (10:1 CH2Cl2:MeOH)