反应详情

To a solution of N5-(4-Iodo-2-methoxy-pyridin-3ylmethylene)-6-methyl-2-morpholin-4-yl-pyrimidine-4,5-diamine (140 mg, 0.31 mmol) in a mixture of MeOH:THF (20 mL:10 mL) was added iodobenzene diacetate (198 mg, 0.62 mmol). After stirring at ambient temperature for 4 hours, the solvents were evaporated in vacuo and the crude was purified by preparative HPLC (see method below) to give the title compound as an amber solid (50 mg, 36%): IR (KBr, cm−1) 3420, 2853, 1618; 1H NMR (400 MHz, CDCl3) δ 9.63 (s, 1H), 7.83 and 7.54 (d, J=5.3, 1H), 3.91 (s, 3H), 3.81-3.77 (m, 8H), 2.72 (s, 3H); LCMS (+ESI, M+H+) m/z 453; HPLC: 97% (220 nm).

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