反应详情

To N1,N1′-((5-(3-(iso-butylamino)propoxy)-1,3-phenylene)bis(methylene))bis(N3-(3-aminopropyl)propane-1,3-diamine) from step 6 was added methanolic HCl (50 mL, 1.0M). The reaction mixture was stirred for 1 h, the reaction mixture was concentrated under reduced pressure and the solid collected by vacuum filtration. The solid was washed with Et2O (10 mL) and hot MeOH (10 mL) to afford the desired product (0.14 g, 43%) as a white solid. 1H NMR (500 MHz, D2O) 6 ppm 7.21 (s, 1H), 7.19 (s, 2H), 4.30 (s, 4H), 4.23 (t, J=5.5 Hz, 2H), 3.29 (t, J=7 Hz, 2H), 3.25-3.19 (m, 12H), 3.12 (t, J=7.5 Hz, 4H), 2.95 (d, J=7 Hz, 2H), 2.25-2.03 (m, 11H), 1.01 (d, J=7.5 Hz, 6H). 13C NMR (125 MHz, D2O) 158.9, 133.0, 123.7, 117.1, 65.8, 54.8, 50.7, 45.7, 44.7, 44.6, 44.2, 36.7, 25.5, 25.2, 23.7, 22.6, 19.1. LRMS [M+H]+494.4.

1. concentrationthe reaction mixture was concentrated under reduced pressure
2. filtrationthe solid collected by vacuum filtration
3. washThe solid was washed with Et2O (10 mL) and hot MeOH (10 mL)