反应详情

温度

80 °C

To a degassed solution of 2-(4-fluorophenyl)-5-iodo-N-methyl-6-(N-methylmethylsulfonamido)furo[2,3-b]pyridine-3-carboxamide (prepared according to International Patent Application Publication No. WO2011131709, 3.0 g, 6 mmol), hypodiboric acid (1.08 g, 1.2 mmol) and KOAc (1.8 g, 1.8 mmol) in EtOH (60 mL) was added Pd(OAc)2 (50 mg) and Ad2n-BuP (50 mg) under nitrogen atmosphere. The reaction mixture was stirred at 80° C. for 5 h, concentrated in vacuo to remove EtOH. The residue was purified by column chromatography (EA:DCM=1:1˜DCM:MeOH=5:1) to afford the desired product of (2-(4-fluorophenyl)-3-(methylcarbamoyl)-6-(N-methylmethylsulfonamido)furo[2,3-b]pyridin-5-yl)boronic acid (1 g, yield: 40%). 1H-NMR (DMSO-d6, 400 MHz) δ 8.53 (d, J=4.4 Hz, 1H), 8.24 (s, 1H), 8.00˜8.04 (m, 3H), 7.40 (t, J=8.8 Hz, 2H), 4.08 (br s, 1H), 3.17 (s, 3H), 3.06 (s, 3H), 2.85 (d, J=4.8 Hz, 3H). MS (M+H)+: 422.

1. concentrationconcentrated in vacuo
2. customto remove EtOH
3. customThe residue was purified by column chromatography (EA:DCM=1:1˜DCM:MeOH=5:1)