反应详情

温度

25 °C

A solution of (12) (0.03 g, 0.071 mmol) in TFA (5 mL) was capped with a drying tube and stirred at 25° C. for 12 h. The reaction mixture was then concentrated to a light brown oily residue (0.033 g, 97.5%); 1H NMR (DMSO) δ 13.00 (br s, 1H), 7.68 (d, 2H, J=8.6), 7.30 (d, 1H, J=8.7), 6.92 (d, 1H, J=2.2), 6.85 (dd, 1H, J=8.0, 2.3), 3.99 (d, 2H, J=13.3), 3.78 (s, 3H), 3.70 (m, 1H), 3.46 (t, 2H, J=11.2), 2.09 (d, 2H, J=10.7), 1.56 (m, 2H); 13C NMR (DMSO) δ 167.4, 156.2, 151.3, 150.0, 131.2, 131.0, 124.0, 117.1, 111.9, 111.3, 110.3, 96.6, 55.7, 47.3, 45.4, 30.2; HRMS (FAB) m/z 367.1777 (M+H)+ (C20H22N4O3 requires 367.1765); Anal. (C20H22N4O3 ·1CF3COOH·3/4H2O) C, H, N.

1. concentrationThe reaction mixture was then concentrated to a light brown oily residue (0.033 g, 97.5%)