反应详情

温度

150 °C

In a microwave tube were charged with compound 11I (29 mg, 0.1 mmol), (3-carbamoyl-4-fluorophenyl)boronic acid (27 mg, 0.15 mmol), LiCl (13 mg, 0.3 mmol), Na2CO3 (17 mg, 0.2 mmol), Pd(PPh3)2Cl2 (3.5 mg, 0.005 mmol). To the mixture was added 2 mL of DME/DMF/H2O (4/1/1). The mixture was heated up to 150° C. for 30 min in a Microwave Synthesizer. After cooled down and filtered through a syringe filter, purified on reverse phase HPLC eluting with acetonitrile and water (with 0.1% TFA) to afford the title product. 1H NMR (400 MHz, CD3OD) δ 8.61 (d, J=8.0 Hz, 1H), 8.07 (s, 1H), 7.48 (dd, J=6.9, 2.3 Hz, 1H), 7.40-7.33 (m, 1H), 7.22 (dd, J=10.7, 8.5 Hz, 1H), 6.70 (t, J=9.2 Hz, 1H), 6.45 (d, J=6.2 Hz, 2H), 5.24 (q, J=7.5 Hz, 1H), 4.76 (s, 2H), 3.85-3.56 (m, 4H), 3.41 (s, 3H), 3.01 (ddd, J=29.2, 13.3, 7.4 Hz, 2H), 2.63-2.34 (m, 4H), 1.88-1.60 (m, 4H). MS (m/z) 676.46 [M+H]+.

1. temperatureAfter cooled down
2. filtrationfiltered through a syringe
3. filtrationfilter
4. custompurified on reverse phase HPLC
5. washeluting with acetonitrile and water (with 0.1% TFA)