反应详情

温度

100 °C

To a rb flask containing ethyl 3-(4-fluoro-3-(2-oxo-2-(4-(1-phenyl-1H-tetrazol-5-yl)piperazin-1-yl)acetyl)-1H-pyrrolo[2,3-c]pyridin-7-yl)-1H-pyrazole-5-carboxylate (0.058 g, 0.10 mmol) in DMF (5 mL) and water (5 mL) was added lithium hydroxide monohydrate (0.044g, 1.05 mmol). The mixture was heated to 100° C. for 21.5 h. The mixture was cooled to rt, and HCl was added to PH=1. Solids precipitated out of solution, and were collected by filtration to give the title compound as a yellow solid (0.03 g). LCMS: m/e 531.15 (M+H)+, ret time 2.10 min (method 2). 1H NMR (500 MHz, DMSO-D6) δ ppm 14.37 (s, 1 H) 13.58 (s, 1 H) 12.23 (s, 1 H) 8.21-8.42 (m, 2 H) 7.52-7.77 (m, 5 H) 7.35 (s, 1 H) 3.08-3.76 (m, 8 H).

1. temperatureThe mixture was cooled to rt
2. customSolids precipitated out of solution
3. filtrationwere collected by filtration