反应详情

温度

25 °C

A solution of 4-[1-(4-Amino-6,7-dimethoxy-quinazolin-2-yl)-piperidin-4-ylamino]-benzoic acid tert-butyl ester (5) (0.55 g, 1.15 mmol) in HCl (10 mL, 1M in 1,4-dioxane) was capped with a drying tube and stirred at 25° C. for 12 h. The reaction mixture was concentrated to give a pale yellow solid residue (0.52 g, 91.3%); 1H NMR (DMSO) δ 12.08 (br s, 2H), 8.85 (br s, 1H), 8.64 (br s, 1H), 7.73 (s, 1H), 7.67 (d, 2H, J=8.7), 7.48 (s, 1H), 6.65 (d, 2H, J=8.8), 6.47 (br s, 1H), 4.51 (d, 2H, J=13.2), 3.88 (s, 3H), 3.84 (s, 3H), 3.71 (m, 1H), 3.35 (t, 2H, J=12.0), 2.06 (d, 2H, J=10.4), 1.47 (m, 2H); 13C NMR (DMSO) δ 167.8, 161.6, 155.7, 151.7, 151.1, 147.1, 136.2, 131.6, 117.1, 111.6, 105.0, 101.7, 99.1, 56.5, 56.4, 48.1, 43.6, 31.2; HRMS (FAB) m/z 424.2003 (M+H)+ (C22H25N5O4 requires 424.1985); Anal. (C22H25N5O4 ·2HCl) C, H, N.

1. concentrationThe reaction mixture was concentrated