反应详情

温度

55 °C

A solution of 1-(3-chloro-phenyl)-2-[2,6-dimethoxy-5-(4-methyl-6-morpholin-4-yl-1H-benzoimidazol-2-yl)-pyrimidin-4-ylamino]-ethanol (0.041 g, 0.078 mmol) in a mixture of AcOH (17.4 M) and HCl (11.6 M: (1.3 mL: 1.0 mL) was stirred in a sealed tube at 55° C. for 18 hours. Then solvents were evaporated in vacuo and the crude material was purified by preparative HPLC (see method below) to give the title compound as a beige solid (29 mg, 77%), HPLC 99%. LCMS (+ESI, M+H+) m/z 497. IR (KBr, cm−1) 3420, 2961, 2856, 1717, 1635, 1559; 1H NMR (400 MHz DMSO) δ 11.88 (s, 2H), 10.84 (s, 1H), 7.58 (s, 1H), 7.46-7.30 (m, 3H), 6.97 (d, J=2 Hz, 1H), 6.68 (s, 1H), 6.10 (br s, 1H), 4.90 (m, 1H), 3.89 (m, 1H), 3.76 (m, 4H), 3.61 (m, 1H), 3.04 (m, 4H), 2.49 (3H, s); HRMS calcd for C24H25ClN6O4:497.1704; found 497.1698.

1. customThen solvents were evaporated in vacuo
2. customthe crude material was purified by preparative HPLC (see method below)