反应详情

To a solution of 1-(4-aminoquinazoline-7-ylmethyl)piperazine-2-one (25 mg, 0.097 mmol), EXAMPLE 72, in 1 mL of DMF is added 4-chloro-benzyl isocyanate (22 mg, 0.13 mmol, prepared as described in EXAMPLE 37). After stirring 1 h at room temperature, the solution is concentrated. The crude product is purified by RP-HPLC eluting in a gradient of 10% CH3CN/H2O (0.1% TFA) to 80% CH3CN/H2O (0.1% TFA) and the appropriate product fractions are combined and lyopholized to provide the title compound (36 mg, 0.067 mmol) as a white solid. 1H NMR (d6-DMSO, 300 MHz) δ9.76 (bs, 2H), 8.83 (s, 1H), 8.38 (d, 1H), 7.64 (d, 1H), 7.60 (s, 1H), 7.34 (d, 2H), 7.31 (m, 1H), 7.26 (d, 2H), 4.75 (s, 2H), 4.22 (d, 2H), 4.08 (s, 2H), 3.60 (m, 2H), 3.35 (m, 2H). ESI MS, [M+H]+=425,427 (Cl pattern).

1. concentrationthe solution is concentrated
2. customThe crude product is purified by RP-HPLC
3. washeluting in a gradient of 10% CH3CN/H2O (0.1% TFA) to 80% CH3CN/H2O (0.1% TFA)