A multi-substituted 1,2,3,4,8,8a-hexahydroquinoline compound and its preparation
A hexahydroquinoline, multi-substitution technology, applied in organic chemistry, drug combination, antineoplastic drugs, etc., can solve the problems of preparation methods and applications that have not been reported in literature, and achieve low cost, fast reaction time, and simple operation Effect
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Embodiment 1
[0033]
[0034] Add K to a microwave tube equipped with a magneton under a nitrogen atmosphere 2 PtCl 4 (20.8mg, 0.05mmol), aminoalkyne I-a (101.5mg, 0.5mmol), chalcone II-a (208.0mg, 1.0mmol), then add 10mL of anhydrous methanol with a syringe, under microwave irradiation, react at 150°C for 10 After 10 minutes, TLC detected that the reaction was complete, and then subjected to silica gel column chromatography (eluent: petroleum ether / ethyl acetate=10:1), to obtain 118 mg of light yellow solid III-aa. 1 H NMR (500MHz, CDCl 3 )δ7.35(d, J=7.2Hz, 2H), 7.28(d, J=7.4Hz, 2H), 7.24(d, J=0.9Hz, 2H), 7.20(dd, J=8.5, 7.0Hz, 3H), 7.15–7.11(m, 1H), 6.98(d, J=8.9Hz, 2H), 6.84(d, J=9.0Hz, 2H), 6.03(d, J=2.1Hz, 1H), 3.79( s,3H),3.60–3.50(m,3H),3.16(ddd,J=16.5,9.0,2.2Hz,1H),2.83(dd,J=16.5,4.9Hz,1H),2.07(d,J= 5.7Hz, 2H), 1.78–1.68(m, 2H); 13 C NMR (125MHz, CDCl 3 )δ155.00,144.89,142.43,140.87,135.92,132.96,128.39,128.25,127.82,126.80,126.33,125.15,124.46,121.91,116.02,114.29,55.52,52...
Embodiment 2
[0037] Add K to a microwave tube equipped with a magneton under a nitrogen atmosphere 2 PtCl 4 (20.8mg, 0.05mmol), aminoalkyne I-a (0.5mmol), chalcone II-b (1.0mmol), then add 10mL of anhydrous methanol with a syringe, and react under microwave irradiation at 79°C for 10 minutes, and the reaction is complete by TLC After silica gel column chromatography (eluent: petroleum ether / ethyl acetate=10:1), 118 mg of light yellow solid was obtained. The structure was confirmed by high-resolution mass spectrometry, HRMS(ESI)[M+H]calculated for[C 30 h 32 NO3] + 454.2377, found 454.2373.
[0038]
Embodiment 3
[0040] Add K to a microwave tube equipped with a magneton under a nitrogen atmosphere 2 PtCl 4 (20.8mg, 0.05mmol), aminoalkyne I-a (0.5mmol), chalcone II-c (1.0mmol), then add 10mL of anhydrous methanol, under microwave irradiation, react at 150°C for 10 minutes, TLC detects that after the reaction is complete, the Silica gel column chromatography (eluent: petroleum ether / ethyl acetate=10:1) gave a pale yellow solid. The structure was confirmed by high-resolution mass spectrometry, HRMS(ESI)[M+H]calculated for[C 30 h 32 NO] + 422.2478, found 422.2478.
[0041]
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