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), (49 mg, 0.13 mmol) in CH3CN (1 mL) was added [(1-(chloromethyl)4-fluoro-1,4-diazoniabicyclo[2.2.2]octane bis(tetrafluoroborate)] (SELECTFLUOR®) (46 mg, 0.13 mmol), and the mixture was stirred at rt for 16 h. The solid was filtered off and the filtrate was subjected to HPLC purification with a gradient elution from 10% to 90% acetonitrile in water to afford 4 mg (8%) of the desired product. 1H NMR (300 MHz, CD2Cl2) δ 8.62 (s, 1H), 7.40 (d, 1H), 7.16-7.35 (m, 4H), 7.05 (dd, 1H), 7.76 (dd, 1H), 3.75 (s, 3H), 2.12 (s, 3H), 1.40 (s, 9H). ES-MS m/z 398.2 (MH+); HPLC RT (min) 4.06.

1. filtrationThe solid was filtered off
2. customthe filtrate was subjected to HPLC purification with a gradient elution from 10% to 90% acetonitrile in water