N-(2-isopropyl) para hydroxybenzene carbonylhydrazone lead complex, and preparation method and application thereof
A kind of technology of lead hydroxybenzoyl hydrazone and hydroxybenzoyl hydrazone, which is applied to N-(2-isopropionic acid) p-hydroxybenzoyl hydrazone lead complex and its preparation and application fields, and can solve the problem of main group metal coordination To avoid problems such as less research on chemical substances, to avoid difficult purification, excellent bacteriostatic properties, and easy operation.
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[0031] The preparation method of N-(2-isopropyl acid) p-hydroxybenzoyl hydrazone lead complex, the steps are as follows:
[0032] (1) N-(2-isopropanoic acid) methyl p-hydroxybenzoate and hydrazine hydrate with a molar ratio of 1:0.5~1:4 are heated and refluxed in an organic solvent for 1~4 hours to obtain N-(2- Isopropyl acid) p-hydroxybenzoyl hydrazide;
[0033] (2) The product obtained in step (1) with a molar ratio of 1:0.5~1:5 and pyruvic acid are heated and refluxed in an organic solvent for 1~6 hours to obtain N-(2-isopropanoic acid) p-hydroxybenzyl Acylhydrazone
[0034] (3) Dissolve the lead salt in water and place it on the bottom of the test tube; then slowly inject an equal volume of mixed solvent into the above test tube; finally, dissolve the product obtained in step (2) in an equal volume of methanol, and adjust the pH with alkali After the value reaches 6-7, it is injected into the test tube, and the target product is obtained after diffusion.
[0035] In step (3), th...
Embodiment 1
[0043] Example 1: Preparation of N-(2-isopropanoic acid) p-hydroxybenzoyl hydrazone
[0044] Preparation of N-(2-isopropanoic acid) p-hydroxybenzoic acid hydrazide: Add 5mmol 4-hydroxybenzoic acid methyl ester, 7.5mmol 85% hydrazine hydrate and 45mL absolute ethanol into a 100mL round bottom flask, stir and reflux in a water bath 3 After hours, transfer it to a beaker while it is hot, and cool it naturally to precipitate a large amount of white crystals. After standing, it is suction filtered and washed with absolute ethanol. The melting point is measured to be 264-265°C, which is consistent with the literature value 264-265°C, and the yield is 80%.
[0045] In a 100 mL round bottom flask, add 1 mL of glacial acetic acid dropwise to 50 mL of absolute ethanol with 10 mmol of N-(2-isopropanoic acid) p-hydroxybenzoyl hydrazide and 25 mmol of pyruvic acid. Stir and reflux in a water bath for 4 hours. After cooling, it was filtered and washed with a small amount of methanol. First, it ...
Embodiment 2
[0047] Example 2: [Pb(C 10 H 9 N 2 O 4 ) 2 ]n Preparation
[0048] Step A: Dissolve 0.1mmol of lead nitrate in 5mL of water, and place it on the bottom of a 20mL test tube after it is completely dissolved;
[0049] Step B: Slowly inject 5 mL of a mixed solvent with a volume ratio of 1:1 into the liquid surface of the solution obtained in Step A with a syringe to form an intermediate layer;
[0050] Step C: Dissolve 0.1 mmol of N-(2-isopropanoic acid) p-hydroxybenzoyl hydrazone in 5 mL of methanol, adjust the pH to 6-7 with a base, and slowly inject it into the liquid surface of the solution obtained in step B with a syringe. Form the upper layer. After standing, after the diffusion reaction, N-(2-isopropanoic acid) p-hydroxybenzoyl hydrazone lead complex is obtained.
[0051] White solid, 42% yield; elemental analysis (C 20 H 18 N 4 O 8 Pb) (%): calculated value: C 36.97, H 2.77, N8.63; measured value: C 36.56, H, 2.65, N, 8.96%. Infrared spectrum analysis (KBr, cm -1 ): 3549(w), 301...
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