2-(2-二环己基磷杂NYL-苯基)-1-甲基-1H-吲哚

在室温和氮气氛下,将N-甲基-2-苯基-3-溴吲哚(0.855 g,3.0 mmol)溶于新鲜蒸馏的THF(20mL)中. 在干冰/丙酮浴中将溶液冷却至-78℃.通过注射器滴加滴定的正丁基锂(3.3mmol). 将反应混合物在-78℃下搅拌30分钟后,加入氯二环己基膦(0.66mL,3.3mmol)的THF(5mL)溶液. 使反应升温至室温并搅拌过夜. 减压除去溶剂. 真空除去溶剂后,将产物依次用冷的MeOH / EtOH混合物洗涤,然后真空干燥. 该产品是2-(2-二环己基磷杂NYL-苯基)-1-甲基-1H-吲哚,白色固体(0.85g,71%). 熔点:122.0-123.2℃. 1 H NMR (400 MHz, C6D6) δ1.19-2.55 (m, 22H), 3.08 (s, 3H), 7.19-7.39 (m, 6H), 7.51 (d, J=7.3 Hz, 2H), 8.16-8.18 (m, 1H); 13 C NMR (100 MHz,CDCl 3) δ 26.8, 27.3, 27.5 (overlapped), 27.6, 30.7 (overlapped), 31.0, 31.1,32.5, 32.8, 34.8, 34.9, 105.1, 105.3, 110.3, 120.5, 122.1 (Overlapped), 127.8, 127.9, 131.3(overlapped), 132.1 (overlapped), 133.3 (overlapped), 138.8 (overlapped), 149.8, 150.2(unresolved complex C-P splittings were observed); 31 P NMR (162 MHz, C6D6) δ-18.36; IR(cm -1) 3049.36, 2921.78, 2845.98, 1465.12, 1443.10, 1372.54, 1336.47, 1264.83, 1106.31,1021.29, 887.02, 849.63, 795.91, 737.94, 698.91, 619.86, 550.50; MS (EI): m/z (relative
intensity) 403(M+, 25), 348 (5), 321 (30), 238 (100), 222 (25), 207 (10); HRMS: calcd. forC27H34NPH + : 404.2507, found 404.2511.
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