反应详情

A solution of 14e (125 mg, 0.25 mmol) in THF (10 mL) was hydrogenated over PtO2 at 50 psi for 2 h. After removal of the catalyst, the solution was concentrated to a small volume under reduced pressure below 25° C. and diluted with iPr2O to give 15e (115 mg, 98%): mp >250° C.; 1H NMR [(CD3)2SO] δ 11.56 (d, J=1.4 Hz, 1 H, NH), 8.08 (d, J=8.5 Hz, 1 H, H-6), 7.76 (d, J=8.2 Hz, 1 H, H-9), 7.70 (s, 1 H, H-4), 7.46 (t, J=7.4 Hz, 1 H, H-8), 7.39 (d, J=8.9 Hz, 1 H, H-7'), 7.28 (t, J=7.7 Hz, 1 H, H-7), 7.17 (d, J=2.2 Hz, 1 H, H-4'), 7.07 (d, J=1.8 Hz, 1 H, H-3'), 6.91 (dd, J=8.9, 2.4 Hz, 1 H, H-6'), 5.98 (s, 2 H, NH2), 4.73 (dd, J=10.6, 9.1 Hz, 1 H, H-2), 4.51 (dd, J=10.9, 1.4 Hz, 1 H, H-2), 4.16-4.08 (m, 1 H, H-1), 4.06 (t, J=5.9 Hz, 2 H, OCH2), 3.98 (dd, J=10.9, 3.0 Hz, 1 H, CHHCl), 3.75 (dd, J=10.9, 8.1 Hz, 1 H, CHHCl), 2.65 (t, J=5.9 Hz, 2 H, OCH2CH2), 2.24 (s, 6 H, N(CH3)2).

1. customAfter removal of the catalyst
2. concentrationthe solution was concentrated to a small volume under reduced pressure below 25° C.
3. additiondiluted with iPr2O