反应详情

The product 2 is treated with fumaric acid in an EtOH/Et2O solution. The fumaric acid salt 3 crystallizes from the reaction medium at 0° C. Mp=175-177° C. 1H NMR (300 MHz, DMSO-d6): δ 13.12 (bs, 2H, OH), 8.70 (bs, 1H, NH), 8.64 (d, 1H, J=4.1 Hz, Harom), 8.03 (d, 2H, J=8.3 Hz, Harom), 7.92 (d, 1H, J=8.0 Hz, Harom), 7.86 (t, 1H, J=8.0 Hz, Harom), 7.70 (s, 1H, Harom), 7.48 (broad d, 2H, J=8.3 Hz, Harom) 7.35-7.31 (m, 1H, Harom) 6.62 (s, 2H, ═CH), 6.51 (bs, 1H, NH), 4.67 (bs, 2H, CH2), 4.51 (bs, 1H, OH), 3.82 (bs, 1H, CH), 3.45-3.32 (m, 2H, CH2), 2.90 (hept, 1H, J=6.8 Hz, CH), 1.65-1.35 (m, 2H, CH2), 1.23 (d, 6H, J=6.8 Hz, 2 CH3), 0.84 (t, 3H, J=7.4 Hz, CH3).

1. customThe fumaric acid salt 3 crystallizes from the reaction medium at 0° C