Benzimidazolamines compounds as well as preparation method and application thereof
A technology of benzimidazolamine and benzimidazole, which is applied in the field of preparation of the compound, can solve problems such as narrow antibacterial spectrum, poor water solubility, and ineffective treatment of non-albicans
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Embodiment 1
[0060] The preparation of embodiment 1,2-chloromethyl-1H-benzimidazole (compound VI)
[0061]
[0062] Add 5.412g (0.050mol) of o-phenylenediamine, 7.114g (0.075mol) of chloroacetic acid and 60mL of 5mol / L hydrochloric acid into a 100mL round bottom flask, heat to reflux for 4 hours, cool, neutralize with ammonia water, and keep stirring until yellow The solid precipitated, was filtered by suction, dried, and recrystallized from absolute ethanol to obtain 7.803 g of compound VI, with a yield of 91.2%; a yellow solid with a melting point of 143-144°C.
Embodiment 2
[0063] Embodiment 2, the preparation of N-((1H-benzimidazol-2-yl)methyl)-2-fluoroaniline (compound I-1)
[0064]
[0065] Add 1.669g (0.010mol) of compound VI, 1.110g (0.010mol) of 2-fluoroaniline and an appropriate amount of ethanol (subject to the complete dissolution of the raw materials) into a 100mL round-bottomed flask, and stir at a temperature of 75-90°C for 24-72 hours. , then add 1.272g (0.012mol) of anhydrous sodium carbonate under stirring conditions, and react at a temperature of 10 to 60°C for 2 to 4 hours. TLC traces until the end of the reaction, and then concentrates, extracts, and separates by column chromatography. After crystallization and drying, 1.764 g of compound I-1 was obtained, with a yield of 73.1%; a yellow solid with a melting point of 164-165°C; 1 H NMR (300MHz, CDCl 3 )δ: 4.60 (s, 2H, benzimidazolyl-CH 2 ), 6.46~6.44(m, H, Benzene-6-H), 6.50(m, H, Benzene-4-H), 6.94~6.91(m, H, Benzene-5-H), 7.17~7.14(m , H, benzene-3-H), 7.27~7.23 (m, 2H, ...
Embodiment 3
[0066] Embodiment 3, the preparation of N-((1H-benzimidazol-2-yl)methyl)-3-trifluoromethylaniline (compound 1-2)
[0067]
[0068] Using compound VI 1.665g (0.010mol), 3-trifluoromethylaniline 1.607g (0.010mol) and anhydrous sodium carbonate 1.272g (0.012mol) as starting materials, according to the method described in Example 2, compound I was prepared -2 2.074g, yield 71.2%; yellow solid, melting point 155-156°C; 1 H NMR (300MHz, CDCl 3 )δ: 4.61 (s, 2H, benzimidazolyl-CH 2 ), 6.74~6.71(d, H, benzene-6-H), 6.82(s, H, benzene-2-H), 7.00~6.97(d, H, benzene-4-H), 7.21~7.19(d , H, benzene-5-H), 7.27~7.24 (m, 2H, benzmidazole-5, 6-H), 7.58~7.55 (m, 2H, benzmidazole-4, 7-H) ppm.
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