反应详情

温度

90 °C

The product of Step 1 (43 mg, 0.11 mmol), 4-pyrazole boronic acid pinacol ester (32 mg, 0.16 mmol), tetrakis palladium triphenylphosphine (13 mg, 0.11 mmol) and sodium tert-butoxide are suspended in a mixture of DMF (2 mL) and water (0.66 mL). The reaction is degassed with nitrogen for 10 min before being sealed and stirred at 90° C. for 16 h. The reaction is condensed in vacuo and the residue purified by column chromatography, eluting with 3% methanolic ammonia (7 N) in dichloromethane to give the title compound as a pale yellow powder (12 mg, 29%). 1H NMR (400 MHz, d6-DMSO) δ 2.48 (s, 4H, CH2CH2), 3.35 (s, 2H, CH2), 3.63 (t, 4H, J=6 Hz, CH2CH2), 6.97 (s, 1H, H), 8.43 (s, 1H, H), 8.61 (brs, 2H), 8.81 (s, 1H, H), 12.9-12.4 (brs, 2H, NH×2). MS (MH+, m/z) 384.

1. customThe reaction is degassed with nitrogen for 10 min
2. custombefore being sealed
3. customcondensed in vacuo
4. customthe residue purified by column chromatography
5. washeluting with 3% methanolic ammonia (7 N) in dichloromethane