3c: 产率80%. m.p. 238~239℃ (232~234℃)[10]; IR (KBr) ν: 3450, 3078, 1657, 1611, 1560, 14517, 1465, 1345, 761 cm−1; 1H NMR (CDCl3) δ: 6.14(s, 1H, CH), 7.28–8.22 (m, 12H,12×CH), 11.40(s, 1H, OH), 11.59(s, 1H, OH); 13C NMR (CDCl3) δ: 36.55, 103.30, 104.80, 116.26, 123.87, 124.52, 125.15, 127.58, 133.35, 143.36, 146.93, 152.40, 164.84, 166.42, 169.10.
3d: 产率96%. m.p. 269~270℃ (271~272℃)[9]; IR (KBr) ν: 3450, 3075, 1670, 1614, 1563, 1510, 1413, 1350, 1308, 764 cm−1; 1H NMR (CDCl3) δ: 2.36(s, 3H, CH3), 6.09(s, 1H, CH), 7.11–8.08 (m, 12H, 12×CH), 11.32(s, 1H, OH), 11.55(s, 1H, OH); 13C NMR (CDCl3) δ: 20.96, 35.90, 104.15, 116.62, 124.39, 124.83, 126.38, 129.34, 132.77, 136.42, 152.31.
3e: 产率91%. m.p. 249~250℃ (245~247℃)[9]; IR (KBr) ν: 3452, 3073, 1671, 1611, 1562, 1507, 1452, 1351, 1306, 1257, 768cm−1; 1H NMR (CDCl3) δ: 3.82(s, 3H, CH3O), 6.07(s, 1H, CH), 6.87–8.08 (m, 12H, 12×CH), 11.32(s, 1H, OH), 11.54(s, 1H, OH); 13C NMR (CDCl3) δ: 35.54, 55.27, 114.05,116.62, 124.38, 124.84, 126.96, 127.63, 132.79, 158.46.
3.结果与讨论
表1是微波辐射功率和反应温度对反应的影响。