反应详情

温度

185 °C

To a dry 15 mL ChemGlass pressure bottle under N2 was added 2-fluoro-4-iodonicotinaldehyde (725 mg, 2.89 mmol), 3-bromo-2-hydrazinylpyridine (543 mg, 2.89 mmol) and anhydrous NMP (Volume: 4.0 mL). The reaction mixture was flushed with argon, securely capped, and heated to 185° C. for 45 min. The reaction mixture was worked up according to the procedure described in Intermediate 69A and the crude product was purified by Biotage Silica gel chromatography using a 12 g Thompson Single Step™ silica cartridge with a linear gradient from 100% CH2Cl2 to 100% ethyl acetate over 11 column volumes to give 867.4 mg (74.9%) of the title compound as a yellow solid. 1H NMR (500 MHz, CCl3D) δ ppm 8.64 (1 H, dd, J=4.58, 1.53 Hz), 8.09-8.25 (3 H, m), 7.65 (1 H, d, J=4.58 Hz), 7.37 (1 H, dd, J=7.93, 4.58 Hz). LC/MS (Condition B): ret. T=3.2 min, (M+H)+ 400.81, 402.81.

1. customThe reaction mixture was flushed with argon
2. customsecurely capped
3. customthe crude product was purified by Biotage Silica gel chromatography