反应详情

To a solution of 2-{[3-tert-butyl-1-(2-methylphenyl)-1H-pyrazol-5-yl]amino}-5-methoxybenzoic acid (Example 4) (130 mg, 0.34 mmol) in DMF (5 mL) were added ammonium chloride (22 mg, 0.41 mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (79 mg, 0.41 mmol), HOBT hydrate (56 mg, 0.41 mmol), and triethylamine (0.17 mL, 1.20 mmol). The reaction mixture was stirred for 16 h and then concentrated under reduced pressure. The residue was purified by HPLC (45-90% acetonitrile in water) to afford the product (63 mg, 49%) as a white solid. 1H NMR (400 MHz, DMSO-d6) δ 1.26 (s, 9H), 1.97 (s, 3H), 3.71 (s, 3H), 6.03 (s, 1H), 7.04 (dd, 1H), 7.24-7.37 (m, 6H), 7.44 (s, 1H), 8.05 (s, 1H), 10.01 (s, 1H); ES-MS m/z 379.3 (MH+); HPLC RT (min) 2.83.

1. concentrationconcentrated under reduced pressure
2. customThe residue was purified by HPLC (45-90% acetonitrile in water)