反应详情

1-{3-[4-(5-Bromothiophen-2-yl)pyrimidin-2-ylamino]-phenyl}-ethanol (15 mg, 0.04 mmol), 2,6-dimethylphenylboronic acid (7.2 mg, 0.048 mmol) and PdCl2(dppf)2 (1.6 mg, 0.002 mmol) were combined in Smith microwave vial (0.2-5.0 mL) in degassed DMA (300 uL) and 2 M Na2CO3 (250 uL). The mixture was micro waved at 165° C. for 900 s. The mixture was diluted with 500 uL DMSO and purified directly by preparative HPLC to afford 1-(3-{4-[5-(2,6-dimethylphenyl)-thiophen-2-yl]-pyrimidin-2-ylamino}-phenylethanol (4.9 mg, 30% yield). 1H NMR (500 MHz, DMSO-d6) δ1.29 (d, J=6.5 Hz, 3H), 2.14 (s, 6H), 4.64 (m, 1H), 5.07 (d, J=3.5 Hz, 1H), 6.91 (d, J=8 Hz, 1H), 7.02 (d, J=4 Hz, 1H), 7.16-7.25 (m, 4H), 7.35 (d, J=5 Hz, 1H), 7.60 (d, J=8 Hz, 1H), 7.84 (br t, 1H), 8.03 (d, J=3.5 Hz, 1H), 8.48 (d, J=5 Hz, 1H), 9.58 (s, 1H). MS: m/z 402 (M+H+).

1. custompurified directly by preparative HPLC