Biguanide derivative, medicinal composition, preparation method of medicinal composition, and application of biguanide derivative or medicinal composition in preparation of antitumor medicines
A technology for biguanide derivatives and drugs, applied in the field of medicine, can solve problems such as unfavorable drug effects, achieve good application prospects, and inhibit proliferation and migration.
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Embodiment 1
[0048] Embodiment 1: the preparation of intermediate 1-(4-trifluoromethyl) phenyl-3-cyanoguanidine
[0049]
[0050] NaN(CN) 2 (50g, 0.56mol) was dissolved in 430mL water to form a solution, and 4-trifluoromethylaniline solution was added at 80°C (dissolve 45g, 0.3mol 4-trifluoromethylaniline in water and concentrated HCl (132mL / 23.5mL)), maintained at 80°C, and continued to react for about 1 hour. White powdery solids gradually precipitated in the reaction solution. TLC detected the reaction solution until no 4-trifluoromethylaniline was contained, that is, the reaction was over. After filtration and vacuum drying, 1-(4-trifluoromethyl)phenyl-3-cyanoguanidine was obtained with a yield of 95.5%.
[0051] Structural validation:
[0052] 1 H NMR (600MHz, DMSO-d 6)δ9.45(s,1H),7.66(d,J=8.5Hz,2H),7.60(d,J=8.5Hz,2H); LC-MS m / z229.0[M+1] + .
Embodiment 2
[0053] Embodiment 2: Preparation of intermediate 1-(3,4-difluoro)phenyl-3-cyanoguanidine
[0054]
[0055] NaN(CN) 2 (50g, 0.56mol) was dissolved in 430mL water to form a solution, and 3,4-difluoroaniline solution was added at 80°C (dissolve 38.7g, 0.3mol 3,4-difluoroaniline in water and concentrated HCl (132mL / 23.5mL)), maintained at 80°C, and continued to react for about 1 hour. Solids gradually precipitated out of the reaction solution. TLC detected the reaction solution until it contained no 3,4-difluoroaniline, that is, the reaction was over. After filtration and vacuum drying, 1-(3,4-difluoro)phenyl-3-cyanoguanidine was obtained with a yield of 95.2%.
[0056] Structural validation:
[0057] 1 H NMR (600MHz, DMSO-d 6 )δ7.50 (d, J = 7.5Hz, 1H), 7.34 (dd, J = 18.0, 8.9Hz, 1H), 7.09 (d, J = 5.8Hz, 1H); LC-MS m / z 197.0[ M+1] + .
Embodiment 3
[0058] Embodiment 3: Preparation of intermediate 1-(2,4-difluoro)phenyl-3-cyanoguanidine
[0059]
[0060] NaN(CN) 2 (50g, 0.5618mob) was dissolved in 430mL water to form a solution, and 2,4-difluoroaniline solution was added at 80°C (dissolve 38.7g, 0.3mol 2,4-difluoroaniline in water and concentrated HCl ( 132mL / 23.5mL)), maintained at 80°C, and continued to react for about 1 hour. Solids gradually precipitated in the reaction solution. TLC detected the reaction solution until no 2,4-difluoroaniline was contained, that is, the reaction was over. After filtration and vacuum drying, 1-(2,4-difluoro)phenyl-3-cyanoguanidine was obtained with a yield of 94.9%.
[0061] Structural validation:
[0062] 1 H NMR (600MHz, DMSO-d 6 )δ8.87(s,1H),7.59(d,J=6.2Hz,1H),7.35–7.29(m,1H),7.07(d,J=8.6Hz,1H); LC-MS m / z194. 8[M-1] - .
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