反应详情

To a solution of 4-(2-fluoro-4-iodophenylamino)-1H-indazole-5-carboxylic acid (70 mg, 0.176 mmol) and N—O-dimethyl-hydroxylamine (21 mg, 0.21 mmol) in DMF (3 mL) was added EDCI (40 mg, 0.21 mmol), HOBt (28 mg, 0.21 mmol) and DIPEA (70 μL, 0.42 mmol). The reaction mixture was stirred at room temperature for 18 hours. The reaction mixture was diluted with ethyl acetate and washed with saturated aqueous sodium hydrogen carbonate then water, dried (Na2SO4), filtered and concentrated in vacuo then azeotroped with diethyl ether to give a pale tan foam (35 mg, 45%). LCMS (Method A): RT=9.63 min, [M+H]+=441. 1H NMR (DMSO-d6, 400 MHz) 13.16 (1 H, s), 8.25 (1 H, s), 7.59-7.51 (2 H, m), 7.34-7.28 (2 H, m), 7.14 (1 H, d, J=8.55 Hz), 6.71 (1 H, t, J=8.73 Hz), 3.38 (3 H, s), 3.10 (3 H, s).

1. washwashed with saturated aqueous sodium hydrogen carbonate
2. dry with materialwater, dried (Na2SO4)
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customthen azeotroped with diethyl ether