Benzo-cycloheptyl-pyridine derivatives containing cyanoguanidine structure, preparation method, and pharmaceutical compositions and medicinal application thereof
A technology of compound and alkyl, applied in drug combination, antipyretic, organic chemistry, etc., can solve the problem of short action time and achieve strong H1 antagonistic effect
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Embodiment 1
[0048]4-(8-Chloro-5H-benzo[5,6]cycloheptane[1,2-b]pyridin-11(6H)-ylidene)-N'-cyano-N-(methylthio) Piperidine-1-amidine (4)
[0049] Deslortadine 6g (0.0193mol), dimethyl dicarboxylate 3g, absolute ethanol 60ml, stirred at room temperature, the solid gradually completely dissolved into a clear liquid, and methyl mercaptan gas was released. After 1 hour, a large amount of white solids were precipitated during the reaction. Continue to react for 1h, filter with suction, and dry to obtain 6.4g of white crystals, mp162-163.5°C, yield 81.2%.
[0050] 1 H NMR (300MHz, CDCl 3 )δ: 2.36-2.44 (m, 2H, CH 2 ), 2.47-2.72 (m, 2H, CH 2 ), 2.75(s, 3H, SMe), 2.78-2.90(m, 2H, CH 2 ), 3.28-3.39 (m, 2H, CH 2 ), 3.50-3.60 (m, 2H, CH 2 ), 4.03-4.15 (m, 2H, CH 2 ), 7.09-7.14(m, 3H, Ar), 7.18(t, 1H, Ar), 7.47(dd, 1H, Ar), 8.40(dd, 1H, Ar)
[0051] IR (cm -1 ): 2929, 2180, 1548, 1540, 1434, 991.
[0052] 4-(8-Chloro-5H-benzo[5,6]cycloheptane[1,2-b]pyridin-11(6H)-ylidene)-N'-cyano-N-butylpipe...
Embodiment 2
[0058] 4-(8-Chloro-5H-benzo[5,6]cycloheptane[1,2-b]pyridin-11(6H)-ylidene)-N'-cyano-N-pentylpiperidine- 1-amidine (I 2 )
[0059] Taking 4-n-pentylamine as raw material, the preparation method is the same as I 1 . A yellow solid was obtained, mp: 155~156°C, yield 37.2%. Anal.calcd for C 26 h 30 ClN 5 : C, 69.70; H, 6.75; N, 15.63. Found C, 69.69; H, 6.81; N, 15.71.
[0060] MS (ESI, 70ev, m / z): 448.2 [M+H] + , 470.1[M+Na] +
[0061] 1 H NMR (300MHz, CDCl 3 )δ: 0.89(t,3H,CH 3 ); 1.25~1.33(m, 4H, 2CH 2 ); 1.52~1.61 (m, 2H, CH 2 ); 2.36~2.39(m, 2H, =C(CH 2 ) 2 ); 2.41~2.81(m, 2H, =C(CH 2 ) 2 ); 2.83~2.84(m, 2H, N(CH 2 ) 2 ); 3.27~3.39 (m, 6H, PhCH 2 , NCH 2 , N(CH 2 ) 2 ); 3.67~3.73 (m, 2H, CH 2 ); 4.82(br, 1H, NH); 7.09~7.17(m, 4H, Ar-H, pyridine-H); 7.48(dd, 1H, J=7.5Hz, pyridine-H); 8.40(dd, 1H, J=3.9Hz, pyridine-H).
[0062] IR (cm -1 ): 3290, 2953, 2928, 2868, 2158, 1573, 1553, 1503, 1435, 1322, 1295, 999, 993, 827, 810
Embodiment 3
[0064] 4-(8-Chloro-5H-benzo[5,6]cycloheptane[1,2-b]pyridin-11(6H)-ylidene)-N'-cyano-N-octylpiperidine- 1-amidine (I 3 )
[0065] Taking 4-n-octylamine as raw material, the preparation method is the same as I 1 . A white solid was obtained, mp: 136~137°C, yield 41.4%. Anal.calcd for C 29 h 36 ClN 5 : C, 71.07; H, 7.40; N, 14.29. Found C, 71.01; H, 7.38; N, 1432.
[0066] MS (ESI, 70ev, m / z): 490.2 [M+H] + , 512.3[M+Na] +
[0067] 1 H NMR (300MHz, CDCl 3 )δ: 0.86(t, 3H, CH 3 ); 1.25~1.26(m, 10H, 5CH 2 ); 1.53~1.57 (m, 2H, CH 2 ); 2.35~2.40(m, 2H, =C(CH 2 ) 2 ); 2.50~2.78(m, 2H, =C(CH 2 ) 2 ); 2.80~2.84(m, 2H, N(CH 2 ) 2 ); 3.24~3.39 (m, 6H, PhCH 2 , NCH 2 , N(CH 2 ) 2 ); 3.65 ~ 3.72 (m, 2H, CH 2 ); 4.88(br, 1H, NH); 7.08~7.16(m, 4H, Ar-H, pyridine-H); 7.46(dd, 1H, J=7.6Hz, pyridine-H); 8.38(dd, 1H, J=3.5Hz, pyridine-H).
[0068] IR (cm -1 ): 3285, 2952, 2920, 2852, 2161, 1571, 1538, 1436, 1329, 1297, 1254, 1174, 1085, 993, 829, 783
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