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at 220℃;Inert atmosphere; |
A mixture of 1 ,3-bis(3-aminophenoxy)benzene (56.55 g, 193.44 mmole, 6 equivalents) and oxydiphthalic dianhydride (10 g , 32.24 mmole) was heated at 220C under intert atmosphere for 1 hour and then at 265C in vacuum. The residue dissolved in 150 ml of ethyl acetate, absorbed onto celite and subjected to partial chromatography purification on silica gel using gradient eluation with mixtures of hexanes and ethyl acetate. Fractions containing pure trimer combined, eluent evaporated using rotary evaporator, the residue dried in vacuum inside glovebox at 150C for 1 hour. Compound 12: 1 H-NMR (DMSO-de, 500 MHz): 5.21 (s, (0709) 4H), 6.16 (dd, 2H, J1 = 8 Hz, J2 = 3 Hz), 6.22 (t, 2H, J = 2 Hz), 6.33 (dd, 2H, J1 = 8 Hz, J2 = 2 Hz), 6.66 (t, 2H, J = 2 Hz), 6.74-6.78 (m, 4H), 6.98 (t, 2H, J= 8 Hz), 7.1 1 (dd, 2H, J1 = 8Hz, J2 = 2 Hz), 7.16 (t, 2H, J = 2Hz), 7.23 (br d, 2H, J = 8 Hz), 7.36 (t, 2H, J = 8 Hz), 7.53 (t, 2H, J = 8 Hz), 7.59-7.52 (m, 4H), 8.04 (d, 2H, J = ). 13C-NMR (DMSO-de, 125 MHz): (0710) 166.5, 166.3, 161 .3, 159.0, 157.7, 157.3, 156.9, 156.0, 134.9, 133.7, (0711) 131.5, 130.7, 130.6, 127.6, 126.56, 125.4, 122.9, 1 18.6, 1 17.9, 1 14.2, 1 14.0, 1 13.4, 1 10.4, 109.4, 106.6, 104.6. |