A kind of pyrazolone vanadyl complex, its preparation method and application, and the single crystal preparation of the pyrazolone vanadyl complex
A technology of pyrazolone vanadyl and furoyl pyrazolone, which is applied in the field of organic complexes, can solve the problems of low anti-PTP1B enzyme activity, instability, poor diabetes treatment effect and the like, and achieves the anti-PTP1B enzyme activity. The effect of improving activity and improving water solubility
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[0031] The invention provides a preparation method of the pyrazolone vanadyl complex, comprising the following steps:
[0032] (1) After mixing 1-phenyl-3-methyl-4-furanoylpyrazolone, salicylhydrazide, ethanol and glacial acetic acid, a substitution reaction is carried out to obtain 1-phenyl-3-methyl-4- Furoylpyrazolone salicylhydrazide Schiff base;
[0033] (2) After mixing the ethanol solution of the 1-phenyl-3-methyl-4-furanoylpyrazolone salicylhydrazine Schiff base and the vanadyl acetylacetonate solution, a coordination reaction is carried out to obtain pyrazoline Ketovanadyl complexes;
[0034] The solvent of the vanadyl acetylacetonate solution is a mixture of methanol and chloroform.
[0035] In the present invention, 1-phenyl-3-methyl-4-furanoylpyrazolone, salicylhydrazide, ethanol and glacial acetic acid are mixed for substitution reaction to obtain 1-phenyl-3-methyl-4-furan Formylpyrazolone salicylhydrazide Schiff base.
[0036] In the present invention, the mas...
Embodiment 1
[0060] Weigh 2.90g of 1-phenyl-3-methyl-4-furanoylpyrazolone and 1.52g of salicylhydrazide in a three-necked flask, add 40ml of ethanol, and react in an oil bath with 2.5ml of glacial acetic acid. at 90°C, condensed and refluxed and stirred for 8 hours, then filtered, dried and recrystallized to obtain a solid that was 1-phenyl-3-methyl-4-furanoylpyrazolone salicylhydrazide Schiff base product.
[0061] The ultraviolet spectrogram of the 1-phenyl-3-methyl-4-furanoyl pyrazolone obtained in this example is as follows figure 1 As shown, the infrared spectrum is shown as figure 2 shown. analyze figure 1 with figure 2 It can be seen that the product obtained in this example is the target product 1-phenyl-3-methyl-4-furanoylpyrazolone salicylhydrazide Schiff base.
[0062] Weigh 0.42g of 1-phenyl-3-methyl-4-furanoylpyrazolone salicylhydrazide Schiff base ligand and dissolve it in 30ml ethanol and place it in a three-necked flask, then add 0.14g dissolved in 10ml methanol and 1...
Embodiment 2
[0065] Weigh 2.50g of 1-phenyl-3-methyl-4-furanoylpyrazolone and 1.7g of salicylhydrazide in a three-necked flask, add 45ml of ethanol, and 3ml of glacial acetic acid react in an oil bath at a temperature of 60°C, reflux and stir for 10 hours, then filter, dry and recrystallize to obtain a solid that is 1-phenyl-3-methyl-4-furanoylpyrazolone salicylhydrazide Schiff base product.
[0066] Weigh 0.35g of 1-phenyl-3-methyl-4-furanoylpyrazolone salicylhydrazide Schiff base ligand dissolved in 25ml of ethanol and place in a three-necked flask, then add 0.12g in 8ml of methanol and 9ml The vanadyl acetylacetonate of chloroform was reacted in an oil bath at a temperature of 50°C, condensed and refluxed and stirred for 20 hours, filtered, and dried to obtain a solid that was 1-phenyl-3-methyl-4-furanoylpyridine Azolinone salicylhydrazide Schiff base vanadyl complex product.
[0067] Store the product of the 1-phenyl-3-methyl-4-furanoylpyrazolone salicylhydrazide Schiff base vanadyl c...
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