Method for synthesizing 2,4,5-three substitutive imidazole ring derivative through enzyme catalysis
A synthesis method and technology of imidazole rings, which are applied in the field of synthesizing 2,4,5-trisubstituted imidazole ring derivatives, can solve the problems of complicated operation and severe reaction conditions, and achieve high reaction yield and mild reaction conditions , The effect of less discharge of three wastes
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Embodiment 1
[0022] Embodiment 1: the synthesis of 2-(2-chloro-phenyl)-4,5-diphenyl-1H-imidazole
[0023] Add about 0.5mmol of benzil, about 0.5mmol of o-chlorobenzaldehyde, about 1.5mmol of ammonium acetate, 3mL of ethanol, about 0.035g of lipase (Lipase AT30) into a 10mL test tube, and shake the reaction at a temperature of 45°C After about 9 hours to the end of the reaction, the clear liquid was collected by centrifugation for precipitation, and the crude product was subjected to silica gel column chromatography (developing solvent: petroleum ether / ethyl acetate=5 / 1) to obtain 0.12 g of the compound, with a yield of 73%.
[0024] Product characterization: Mp: 197.2-197.5℃. IR(KBr) 3411, 2812, 1592, 1383, 1357, 1078, 764.1H NMR (400MHz, CDCl3), δ7.31-7.47(m, 10H), 7.53-7.67( m,4H).
Embodiment 2
[0025] Example 2: Synthesis of 2-(2-chloro-phenyl)-4,5-diphenyl-1H-imidazole
[0026] Add about 0.5mmol of benzil, about 0.5mmol of o-chlorobenzaldehyde, about 1.5mmol of ammonium acetate, 3mL of ethanol, and about 0.035g of α-Amylase from Aspergillus oryzae into a 10mL test tube. Shake the reaction at 45°C for about 9 hours until the end of the reaction, centrifuge the clear liquid to precipitate the solvent, and the crude product is subjected to silica gel column chromatography (developing solvent: petroleum ether / ethyl acetate=5 / 1) to obtain 0.075g of the compound with a yield of 45 %.
[0027] Product characterization: Mp: 197.2-197.5℃. IR(KBr) 3411, 2812, 1592, 1383, 1357, 1078, 764.1H NMR (400MHz, CDCl3), δ7.31-7.47(m, 10H), 7.53-7.67( m,4H).
Embodiment 3
[0028] Example 3: Synthesis of 2-(2-chloro-phenyl)-4,5-diphenyl-1H-imidazole
[0029] Add about 0.5mmol of benzil, about 0.5mmol of o-chlorobenzaldehyde, about 1.5mmol of ammonium acetate, 3mL of ethanol, and about 0.035g of α-Amylase from Aspergillus oryzae into a 10mL test tube. Shake the reaction at 30°C for about 9 hours until the end of the reaction, centrifuge the clear liquid to precipitate the solvent, and the crude product is subjected to silica gel column chromatography (developing solvent: petroleum ether / ethyl acetate=5 / 1) to obtain 0.098g of the compound with a yield of 60 %.
[0030] Product characterization: Mp: 197.2-197.5℃. IR(KBr) 3411, 2812, 1592, 1383, 1357, 1078, 764.1H NMR (400MHz, CDCl3), δ7.31-7.47(m, 10H), 7.53-7.67( m,4H).
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