Arylpiperazine compound as well as preparation method and application thereof
A compound, cyano technology, applied in the field of medicine, can solve the problems of incurable prostate cancer, inability to improve treatment results or survival rate, etc.
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Embodiment 1
[0083] Embodiment 1: the preparation of intermediate 5
[0084]
[0085] Add 100mg (0.22mmol) intermediate 4, 59.8mg (0.26mmol) 1-(4-trifluoromethylphenyl) piperazine, 182mg (1.32mmol) potassium carbonate, 15mL acetonitrile in 25mL round bottom flask, at 86 The reaction was carried out at ℃ for 16 h, and TLC showed that the reaction of the starting material was complete. The reaction was stopped, filtered and concentrated. The crude product was purified by silica gel column chromatography, eluent: V (ethyl acetate): V (petroleum ether) = 1:3, to obtain 35.2 mg of white solid, yield: 33%. M.p.:165-166℃; MS(ESI,m / z):509.2[M+1] + ; 8.01(d, J=8.7Hz, 1H), 7.35(d, J=8.0Hz, 2H), 7.26(d, J=3.6Hz, 2H), 7.00–6.94(m, 2H), 6.90(d, J=4.3Hz, 2H), 6.88(dd, J=4.7, 1.9Hz, 1H), 6.78(d, J=2.3Hz, 1H), 5.08(s, 2H), 3.16(t, J=4.9Hz, 4H), 2.92(t, J=6.0Hz, 2H), 2.87(dd, J=9.7, 6.5Hz, 2H), 2.71(t, J=4.9Hz, 4H), 2.68(dd, J=9.8, 6.6 Hz, 2H), 2.61(t, J=6.5Hz, 2H), 2.11(t, J=6.4Hz, 2H); 13 C NMR ...
Embodiment 2
[0086] Embodiment 2: the preparation of compound 6
[0087]
[0088] The reaction of intermediate 4 with 1-(2,5-dimethylphenyl)piperazine, the synthesis process and test conditions are the same as in Example 1. 41.2 mg of white solid was obtained, yield: 40%. M.p.:145-146℃; MS(ESI,m / z):469.2[M+1] + ; 1 HNMR (500MHz, CDCl 3 )δinppm: 8.01(d, J=8.7Hz, 1H), 7.35(d, J=8.0Hz, 2H), 7.26(d, J=3.6Hz, 2H), 7.00–6.94(m, 2H), 6.90( d, J=4.3Hz, 2H), 6.88(dd, J=4.7, 1.9Hz, 1H), 5.08(s, 2H), 3.16(t, J=4.9Hz, 4H), 2.92(t, J=6.0 Hz, 2H), 2.87(dd, J=9.7, 6.5Hz, 2H), 2.71(t, J=4.9Hz, 4H), 2.68(dd, J=9.8, 6.6Hz, 2H), 2.61(t, J =6.5Hz, 2H), 2.11(t, J=6.4Hz, 2H), 1.67(m, 6H); 13 C NMR (126MHz, CDCl 3 )δin ppm:197.21,175.15,162.73,150.96,146.95,139.92,136.18,134.14,130.8,129.69,129.22,129.08,127.80,126.51,123.97,119.81,113.68,113.59,77.28,77.02,76.77,69.91,59.98, 53.35, 51.09, 38.90, 32.62, 30.16, 23.36, 21.74, 21.18, 17.43.
Embodiment 3
[0089] Embodiment 3: the preparation of compound 7
[0090]
[0091] The reaction of intermediate 4 with 1-(3-methylphenyl)piperazine, the synthesis process and test conditions are the same as in Example 1. 64.9 mg of white solid was obtained, yield: 65%. M.p.:132-133℃; MS(ESI,m / z):455.1[M+1] + ; 1 H NMR (500MHz, CDCl 3 )δinppm: 8.01(d, J=8.7Hz, 1H), 7.35(d, J=8.0Hz, 2H), 7.26(d, J=3.6Hz, 2H), 7.00–6.94(m, 2H), 6.90( d, J=4.3Hz, 2H), 6.88(dd, J=4.7, 1.9Hz, 1H), 6.78(d, J=2.3Hz, 1H), 5.08(s, 2H), 3.16(t, J=4.9 Hz, 4H), 2.92(t, J=6.0Hz, 2H), 2.87(dd, J=9.7, 6.5Hz, 2H), 2.71(t, J=4.9Hz, 4H), 2.68(dd, J=9.8 , 6.6Hz, 2H), 2.61(t, J=6.5Hz, 2H), 2.11(t, J=6.4Hz, 2H), 1.62(m, 3H); 13 C NMR (126MHz, CDCl 3 )δin ppm:197.16,162.73,151.31,146.93,140.36,138.80,134.01,129.68,129.06,128.96,127.74,126.51,120.70,116.95,113.67,113.59,113.22,77.28,77.23,77.03,76.77,69.93,60.33, 53.25, 49.19, 38.90, 33.25, 30.16, 23.36, 21.78.
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