A kind of 2-indol-3-yl-quinoline compound with antitumor activity and its preparation method and application
A technology of compounds and quinolines, which is applied in the field of 2-indol-3-yl-quinolines and their preparation, can solve the problems of cumbersome operation steps, low economic efficiency of atoms and steps, and achieve cheap and easy raw materials. High yield, novel structure, less by-products
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Embodiment 1
[0059] Mix 1.0 mmol tetrahydroquinoline, 0.5 mmol indole, cuprous chloride with tetrahydroquinoline quality 10%, trifluoromethanesulfonic acid and 2.5ml toluene with tetrahydroquinoline quality 50%, and mix under oxygen condition Stir the reaction at 80°C for 5 hours, cool to room temperature after the reaction, dilute the reaction solution, filter, take the filtrate, and remove the solvent by rotary evaporation under reduced pressure to obtain the crude product, which is purified by column chromatography to obtain the product 1a, the product It is a yellow solid with a yield of 84% and a purity of 97%.
[0060] The preparation route is:
[0061]
[0062] The structural characterization data of the obtained product 1a are as follows:
[0063] 1 H NMR (400MHz, CDCl 3 )δ8.78(s,1H),8.62(d,J=7.8Hz,1H),8.11(d,J=8.4Hz,1H),8.03(d,J=8.6Hz,1H),7.82–7.66( m,3H),7.62(t,J=7.6Hz,1H),7.39(t,J=7.4Hz,1H),7.28(d,J=7.7Hz,1H),7.24–7.14(m,2H);
[0064] 13 C NMR (101MHz, CDCl 3 )δ155.13,...
Embodiment 2
[0068] 0.9 mmol 6-methyltetrahydroquinoline, 0.5 mmol indole, 6-methyltetrahydroquinoline quality 20% copper chloride, 6-methyltetrahydroquinoline quality 60% methanesulfonic acid Mix with 2.0ml of toluene, stir and react at 160°C under oxygen for 5 hours, cool to room temperature after the reaction, dilute the reaction solution, filter, take the filtrate, and remove the solvent by rotary evaporation under reduced pressure to obtain the crude product, which is passed through the column Chromatographic purification yielded product 2a as a yellow solid with a yield of 88% and a purity of 97%.
[0069] The preparation route is:
[0070]
[0071] The structural characterization data of the resulting product 2a are as follows:
[0072] 1 H NMR (400MHz, DMSO) δ11.66(s, 1H), 8.98–8.89(m, 1H), 8.32(s, 1H), 8.12(d, J=8.6Hz, 1H), 8.00(d, J= 8.6Hz, 1H), 7.96(d, J=8.5Hz, 1H), 7.60(s, 1H), 7.56–7.48(m, 2H), 7.24(dd, J=4.9, 2.0Hz, 2H), 2.46( s,3H);
[0073] 13 C NMR (101MHz, DMSO) ...
Embodiment 3
[0077] 0.75 mmol 7-methyltetrahydroquinoline, 0.5 mmol indole, 7-methyltetrahydroquinoline quality 20% copper acetate, 7-methyltetrahydroquinoline quality 10% p-toluenesulfonic acid Mix with 1.5ml of toluene, stir and react at 130°C under oxygen for 10 hours, cool to room temperature after the reaction, dilute the reaction solution, filter, take the filtrate, and remove the solvent by rotary evaporation under reduced pressure to obtain the crude product, which is passed through the column Chromatographic purification yielded product 3a as a yellow solid with a yield of 85% and a purity of 97%.
[0078] The preparation route is:
[0079]
[0080] The structural characterization data of the obtained product 3a are as follows:
[0081] 1 H NMR(400MHz,DMSO)δ11.72(s,1H),8.96(dd,J=5.7,2.9Hz,1H),8.34(s,1H),8.17(d,J=8.6Hz,1H),7.98 (d,J=8.6Hz,1H),7.88(s,1H),7.75(d,J=8.2Hz,1H),7.54(dd,J=5.8,2.8Hz,1H),7.30(d,J= 8.2Hz, 1H), 7.26(dd, J=5.8, 2.8Hz, 2H), 2.54(s, 3H);
[0082] 13 C N...
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