1-(Benzotriazole-1-methyl)-1-(2,4-dimethylimidazole) zinc complex and its preparation method
A technology of benzotriazole and dimethylimidazole, applied in the field of medicine, can solve the problems of high toxicity, low oxidation resistance, low absorption rate, etc., and achieve strong scavenging effect, simple preparation method and low production cost. Effect
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Embodiment 1
[0033] The preparation method of ligand 1-(benzotriazole-1-methyl)-1-(2,4-dimethylimidazole) of the present invention comprises the following steps:
[0034] (1) Mix 50mmol of benzotriazole with 15mL of water and 15mL of formaldehyde, heat in a water bath to 80°C and reflux for 60min, cool and filter to obtain a white needle-like product, and then recrystallize with ethyl acetate to obtain a white crystal, which is methylol benzotriazole;
[0035] (2) Weigh 25mmol of hydroxymethylbenzotriazole and add it into a single-necked bottle, then add 12.5mL of thionyl chloride dropwise, mix and stir for 20min after the dropwise addition, and reflux at 80°C for 180min; use a rotary evaporator to evaporate the remaining chlorine sulfoxide, to obtain yellow-white crystals, which is chloromethylbenzotriazole;
[0036] (3) Dissolve 20mmol of 2,4-dimethylimidazole in 10mL of DMSO, then add 40mmol of crushed NaOH, heat to 60°C, add 20mmol of chloromethylbenzotriazole, heat in a water bath at...
Embodiment 2
[0040] The preparation method of 1-(benzotriazole-1-methyl)-1-(2,4-dimethylimidazole) zinc complex comprises the following steps:
[0041] (1) Accurately weigh 0.02mmol of zinc chloride and dissolve it in 4mL of methanol to obtain a zinc salt solution;
[0042] (2) Accurately weigh 0.02 mmol of the ligand 1-(benzotriazole-1-methyl)-1-(2,4-dimethylimidazole), dissolve it in 4 mL of methanol, and obtain a ligand solution;
[0043] (3) Add the ligand solution into the zinc salt solution, mix well, filter, add methanol to the filtrate to 10mL, and let it stand at room temperature until colorless rectangular crystals are precipitated.
[0044] The experimental conditions and results of the X-ray single crystal diffraction structure of the complex of the present invention are as follows:
[0045] A single crystal sample with a better crystal form is selected, and X-ray diffraction experiments are carried out on an Xcalibur, Gemini CCD single crystal diffractometer, and the Mo-kα ray ...
Embodiment 3
[0049] The preparation method of 1-(benzotriazole-1-methyl)-1-(2,4-dimethylimidazole) zinc complex comprises the following steps:
[0050] (1) Accurately weigh 0.03mmol of zinc chloride and dissolve it in 4mL of water to obtain a zinc salt solution;
[0051] (2) Accurately weigh 0.03 mmol of the ligand 1-(benzotriazole-1-methyl)-1-(2,4-dimethylimidazole), dissolve it in 6 mL of methanol, and obtain a ligand solution;
[0052] (3) Add the ligand solution into the zinc salt solution, mix well, filter, add methanol to the filtrate to 12mL, and let stand at room temperature until colorless rectangular crystals are precipitated.
[0053] The single crystal structure of the as-prepared azacyclic transition metal zinc complex is shown in figure 1 , 2 , the complex belongs to the monoclinic crystal system, the C1 space group, and the unit cell parameter a is b for c for α is 90°, β is 93.994(2)°, γ is 90°, and the volume V is Z is 4 and the density is 1.482Mg m -3 , θ is 3....
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