反应详情

To a solution of compound 47b (90.0 mg, 0.172 mmol) in DCM (2 mL) was added a solution of methanesulfonic acid as a 1 M DCM solution (0.172 mL, 0.172 mmol). The reaction mixture was stirred at rt for 30 min and then concentrated under reduced pressure to obtain the title compound 126. 1H-NMR (400 MHz, CD3OD) δ (ppm): 2.71 (s, 6H), 3.19-3.26 (m, 4H), 3.85-3.91 (m, 8H), 4.43 (br. s., 4H), 5.60 (s, 2H), 6.83 (d, J=9.0 Hz, 1H), 6.88 (d, J=8.8 Hz, 1H), 7.32 (s, 1H), 7.33-7.38 (m, 1H), 7.56 (td, J=7.7, 1.5 Hz, 1H), 7.63-7.70 (m, 2H), 7.73 (d, J=8.6 Hz, 1H), 7.79 (s, 1H), 7.98 (d, J=8.8 Hz, 1H), 8.26 (d, J=2.4 Hz, 1H). Mass Spectrum (LCMS, ESI pos.) Calcd. for C29H30N8O2: 523.2 (M+H). Found 523.3.

1. concentrationconcentrated under reduced pressure