CN104311604B - Metal cobalt compound as well as preparation method and application thereof - Google Patents
Metal cobalt compound as well as preparation method and application thereof Download PDFInfo
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- CN104311604B CN104311604B CN201410520605.3A CN201410520605A CN104311604B CN 104311604 B CN104311604 B CN 104311604B CN 201410520605 A CN201410520605 A CN 201410520605A CN 104311604 B CN104311604 B CN 104311604B
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- metal cobalt
- pyridine radicals
- cobalt complex
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- 239000002184 metal Substances 0.000 title claims abstract description 40
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 150000001869 cobalt compounds Chemical class 0.000 title abstract 5
- 238000000034 method Methods 0.000 claims abstract description 13
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 5
- 150000004700 cobalt complex Chemical class 0.000 claims description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 26
- 230000000844 anti-bacterial effect Effects 0.000 claims description 23
- 239000000047 product Substances 0.000 claims description 21
- 239000013078 crystal Substances 0.000 claims description 17
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 239000002904 solvent Substances 0.000 claims description 15
- FJKROLUGYXJWQN-UHFFFAOYSA-N 4-hydroxybenzoic acid Chemical compound OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 claims description 12
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 12
- PVNIIMVLHYAWGP-UHFFFAOYSA-N Niacin Chemical compound OC(=O)C1=CC=CN=C1 PVNIIMVLHYAWGP-UHFFFAOYSA-N 0.000 claims description 10
- 235000019441 ethanol Nutrition 0.000 claims description 10
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Substances ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 claims description 7
- 229960000583 acetic acid Drugs 0.000 claims description 6
- 229940088710 antibiotic agent Drugs 0.000 claims description 6
- 239000012362 glacial acetic acid Substances 0.000 claims description 6
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical group OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 5
- 229940090248 4-hydroxybenzoic acid Drugs 0.000 claims description 5
- 229910006124 SOCl2 Inorganic materials 0.000 claims description 5
- 238000007171 acid catalysis Methods 0.000 claims description 5
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 5
- 239000012043 crude product Substances 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 229960003512 nicotinic acid Drugs 0.000 claims description 5
- 235000001968 nicotinic acid Nutrition 0.000 claims description 5
- 239000011664 nicotinic acid Substances 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 238000007363 ring formation reaction Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 4
- 238000001953 recrystallisation Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 229960003350 isoniazid Drugs 0.000 claims description 2
- QRXWMOHMRWLFEY-UHFFFAOYSA-N isoniazide Chemical compound NNC(=O)C1=CC=NC=C1 QRXWMOHMRWLFEY-UHFFFAOYSA-N 0.000 claims description 2
- 230000001954 sterilising effect Effects 0.000 abstract description 11
- 238000004659 sterilization and disinfection Methods 0.000 abstract description 4
- 239000003242 anti bacterial agent Substances 0.000 abstract 2
- -1 3-(4-pyridyl)-5-(3-pyridyl)-1,2,4-triazolyl Chemical group 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 241000191967 Staphylococcus aureus Species 0.000 description 6
- 244000063299 Bacillus subtilis Species 0.000 description 5
- 235000014469 Bacillus subtilis Nutrition 0.000 description 5
- 241000588724 Escherichia coli Species 0.000 description 5
- 241000589517 Pseudomonas aeruginosa Species 0.000 description 5
- 229910017052 cobalt Inorganic materials 0.000 description 5
- 239000010941 cobalt Substances 0.000 description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 238000002347 injection Methods 0.000 description 5
- 239000007924 injection Substances 0.000 description 5
- 241000193830 Bacillus <bacterium> Species 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 239000003814 drug Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- GLDQAMYCGOIJDV-UHFFFAOYSA-N 2,3-dihydroxybenzoic acid Chemical compound OC(=O)C1=CC=CC(O)=C1O GLDQAMYCGOIJDV-UHFFFAOYSA-N 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- UIAFKZKHHVMJGS-UHFFFAOYSA-N beta-resorcylic acid Natural products OC(=O)C1=CC=C(O)C=C1O UIAFKZKHHVMJGS-UHFFFAOYSA-N 0.000 description 3
- 238000012937 correction Methods 0.000 description 3
- 238000002447 crystallographic data Methods 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 3
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000000845 anti-microbial effect Effects 0.000 description 2
- 230000004071 biological effect Effects 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000002775 capsule Substances 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 150000002391 heterocyclic compounds Chemical class 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000006187 pill Substances 0.000 description 2
- ATBIAJXSKNPHEI-UHFFFAOYSA-N pyridine-3-carbonyl chloride Chemical compound ClC(=O)C1=CC=CN=C1 ATBIAJXSKNPHEI-UHFFFAOYSA-N 0.000 description 2
- 239000000375 suspending agent Substances 0.000 description 2
- 239000003826 tablet Substances 0.000 description 2
- 150000003852 triazoles Chemical class 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- NSPMIYGKQJPBQR-UHFFFAOYSA-N 4H-1,2,4-triazole Chemical class C=1N=CNN=1 NSPMIYGKQJPBQR-UHFFFAOYSA-N 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- 241000192023 Sarcina Species 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 230000000843 anti-fungal effect Effects 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 229940121375 antifungal agent Drugs 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000003385 bacteriostatic effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000004696 coordination complex Chemical class 0.000 description 1
- 150000005205 dihydroxybenzenes Chemical class 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 210000002429 large intestine Anatomy 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000000052 vinegar Substances 0.000 description 1
- 235000021419 vinegar Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F15/00—Compounds containing elements of Groups 8, 9, 10 or 18 of the Periodic System
- C07F15/06—Cobalt compounds
- C07F15/065—Cobalt compounds without a metal-carbon linkage
Abstract
The invention discloses a metal cobalt compound as well as a preparation method and an application thereof. The structural formula of the metal cobalt compound is as follows: the chemical name is di(3-(4-pyridyl)-5-(3-pyridyl)-1,2,4-triazolyl) dihydroxy-benzoic cobalt (II), the molecular formula is C38H28CoN10O6, and the relative molecular weight is 779.63. The method for preparing the metal cobalt compound is high in synthesis rate; and moreover, the metal cobalt compound can be used for preparing antibacterial agents, and the prepared antibacterial agents are high in sterilization property and high in sterilization rate.
Description
Technical field
The present invention relates to technical field of medical chemistry, and in particular to a kind of metal cobalt complex and preparation method thereof, and
Its application in medicine is prepared.
Background technology
Metal complex is not only the important object of study of inorganic chemistry, structural chemistry, also as have anticancer, sterilization,
The wide biological activity such as antiinflammatory and paid close attention to by people.Cobalt is biological element particularly important in life sciences, and cobalt is matched somebody with somebody
Compound all has potential using value in the numerous areas such as chemistry, biology, medicine.Experiment shows that cobalt complex is to green pus bar
Bacterium, staphylococcus aureuses, sarcina and escherichia coli have stronger bacteriostasis property.And in existing numerous heterocyclic compounds
In thing, 1,2,4- triazole derivative quite receives always the green grass or young crops of people due to the biological activity and wide application prospect of its wide spectrum
Look at.This heterocyclic compounds mostly has sterilization, antifungal isoreactivity.Therefore the present invention is first with 3- (4- pyridine radicals) -5- (3-
Pyridine radicals) -1,2,4- triazoles and P-hydroxybenzoic acid are part, synthesizing new metal cobalt complex.
The content of the invention
It is an object of the present invention to provide a kind of metal cobalt complex.It is high that another purpose is to provide a kind of synthetic ratio
Method is preparing the metal cobalt complex, and the metal cobalt complex can be applied in antibacterials are prepared, and make to be prepared into
Antibacterials have stronger bactericidal properties and higher sterilizing rate.
In order to solve above-mentioned technical problem, the invention provides a kind of metal cobalt complex and its preparation method and application.
It is as follows that the step of preparing metal cobalt complex includes：
1) by nicotinic acid in SOCl2In be heated to reflux stir 4-5 hour, be evaporated under reduced pressure solvent after obtained by white solid be dissolved in
In chloroform, add and flow back after Isoniazid 5-6 hour, gained material ethyl alcohol recrystallization after solvent is evaporated under reduced pressure and obtains 3- pyridines
Base -4- pyridine radicals imines, and products therefrom is dissolved in ethanol solution, it is anti-with hydrazine hydrate cyclization finally under glacial acetic acid catalysis
Should, flow back 8h, gained crude product chloroform or recrystallizing methanol after solvent is evaporated under reduced pressure and obtains part 3- (4- pyridine radicals) -5- (3-
Pyridine radicals) -1,2,4- triazoles；
2) with 3- (4- pyridine radicals) -5- (3- pyridine radicals) -1,2,4- triazoles and P-hydroxybenzoic acid are part and cobaltous acetate
Capping is carried out at a temperature of 120-200 DEG C, there are reddish-orange crystals to be formed after 48-72h, Jing X- single crystal diffractions are accredited as mesh
Mark product, the target product is the metal cobalt complex of the present invention.
Preferably, the step 2) capping be in autoclave heat pressurization reaction.
The structural formula of the metal cobalt complex of the present invention being prepared into by said method is：
The chemical name of the metal cobalt complex is：Two (3- (4- pyridine radicals) -5- (3- pyridine radicals) -1,2,4- triazolyls)
Resorcylic acid closes cobalt (II)；
The molecular formula of the metal cobalt complex is：C38H28CoN10O6；
The relative molecular weight of the metal cobalt complex is：779.63.
The metal cobalt complex can apply prepare antibacterials in, such as make injection, tablet, pill, capsule,
One or more antimicrobial in suspending agent or Emulsion.
Beneficial effects of the present invention：The metal cobalt complex of the present invention has more stable antibacterial activity and using value,
And the preparation method synthetic ratio of the present invention is high, side-product is few, in being effectively applied to preparation antibacterials, and can be to large intestine bar
Bacterium, staphylococcus aureuses, bacillus subtilises, aerogenesis folder film bacillus, bacillus pyocyaneus etc. produce very high inhibition effect, reach very
High sterilizing rate.
Description of the drawings
Fig. 1 is the method route schematic diagram that the present invention prepares the metal cobalt complex；
Fig. 2 is the x-ray crystal structure schematic diagram consistent with the crystal structure of metal cobalt complex of the present invention, Fig. 2
In the atom that do not mark be carbon atom C or hydrogen atom H.
Specific embodiment
With reference to embodiment, the present invention is described in further detail, to make those skilled in the art with reference to description
Word can be implemented according to this.
Embodiment 1
Fig. 1 is the method route schematic diagram that the present invention prepares the metal cobalt complex.With reference to Fig. 1, metallic cobalt of the present invention
The preparation method of coordination compound is comprised the following specific steps that：
1) 1.23g or 10mmol nicotinic acid is placed in 30ml SOCl2 and is heated to reflux stirring 5 hours, solvent is evaporated under reduced pressure,
The nicotinoyl chlorine of white solid is obtained, product is dissolved in without isolation in 30ml chloroforms, add and continue back after 1.22g or 10mmol Isoniazids
Stream 5 hours, is evaporated under reduced pressure gained material ethyl alcohol recrystallization after solvent and obtains 0.72g 3- pyridine radicals -4- pyridine radicals imines；Will
Products therefrom is dissolved in 30ml ethanol solution, sequentially adds 3-4 drops glacial acetic acid and 3ml hydrazine hydrates, under glacial acetic acid catalysis, with
Hydrazine hydrate ring closure reaction, flow back 8h, gained crude product chloroform or recrystallizing methanol after solvent is evaporated under reduced pressure part 3- (4- are obtained
Pyridine radicals) -5- (3- pyridine radicals) -1,2,4- triazoles, the step obtains the total recovery of part and can reach 32%；
2) by the triazoles of 0.11g or 0.5mmol 3- (4- pyridine radicals) -5- (3- pyridine radicals) -1,2,4- and 0.069g or
0.5mmol P-hydroxybenzoic acid is that part carries out capping with 0.25g or 1mmol cobaltous acetate at 160 DEG C, there is orange after 72h
Red crystals are formed, and Jing X- single crystal diffractions are accredited as target product, and the target product is metal cobalt complex of the present invention, chemistry
Entitled two (3- (4- pyridine radicals) -5- (3- pyridine radicals) -1,2,4- triazolyls) resorcylic acid closes cobalt (II), its molecular formula
For C38H28CoN10O6, its relative molecular weight is 779.63.
Target product X ray crystal structure is determined below：Choose size and be about 0.40mm × 0.20mm × 0.12mm's
Monocrystalline is placed on the CCD X-ray single crystal diffractometers of Brucker SMART 1000 and carries out diffraction, with Jing graphite monochromator monochromatizations
Mo K alpha raysFor incident wavelength, with ω/2 scan mode in the range of 3.01 ° to 25.24 °
Diffraction data 10129 is collected, wherein 3264 is independent point (R (int)=0.0892).The equal Jing Lp factors of total data and
Empirical absorption correction.Solved by direct method using SHELXS-97 programs, obtain its structure chart as shown in Fig. 2 its structure and target
Product is consistent.
The above-mentioned metal cobalt complex being prepared into is made into antibacterial injection needle, and antibacterial examination is carried out according to GB15979-2002
Test, antibacterial injection needle plays very strong bactericidal properties to escherichia coli, staphylococcus aureuses, bacillus subtilises, sterilizing rate reaches
To more than 99%；Film bacillus is pressed from both sides to aerogenesis and bacillus pyocyaneus play certain bactericidal properties, sterilizing rate reaches 80-90%.
Embodiment 2
Fig. 1 is the method route schematic diagram that the present invention prepares the metal cobalt complex.With reference to Fig. 1, metallic cobalt of the present invention
The preparation method of coordination compound is comprised the following specific steps that：
1) 2.46g nicotinic acid is heated to reflux in 60ml SOCl2 stirring 4 hours, gained white after solvent is evaporated under reduced pressure
Solid is dissolved in 60ml chloroforms, is added and flow back after 2.44g Isoniazids 6 hours, and gained material ethanol after solvent is evaporated under reduced pressure
1.41g3- pyridine radicals -4- pyridine radicals imines is recrystallized to give, and by products therefrom in 60ml ethanol solution, finally in ice vinegar
Under acid catalysiss, with 6ml hydrazine hydrate ring closure reactions, flow back 8h, gained crude product recrystallizing methanol after solvent is evaporated under reduced pressure and is matched somebody with somebody
Body 3- (4- pyridine radicals) -5- (3- pyridine radicals) -1,2,4- triazoles, step obtains the total recovery of part and can reach 31%；
2) it is with 0.22g 3- (4- pyridine radicals) -5- (3- pyridine radicals) -1,2,4- triazoles and 0.138g P-hydroxybenzoic acid
Part carries out capping with 0.5g cobaltous acetate at a temperature of 120 DEG C, has reddish-orange crystals to be formed after 48h, and Jing X- monocrystalline spreads out
Penetrate and be accredited as target product.The target product is the metal cobalt complex of the present invention, and its chemical name is two (3- (4- pyridines
Base) -5- (3- pyridine radicals) -1,2,4- triazolyls) resorcylic acid conjunction cobalt (II), its molecular formula is C38H28CoN10O6, its phase
It is 779.63 to molecular weight.
Target product X ray crystal structure is determined below：Choose size and be about 0.40mm × 0.20mm × 0.12mm's
Monocrystalline is placed on the CCD X-ray single crystal diffractometers of Brucker SMART 1000 and carries out diffraction, with Jing graphite monochromator monochromatizations
Mo K alpha raysFor incident wavelength, with ω/2 scan mode in the range of 3.01 ° to 25.24 °
Diffraction data 10129 is collected, wherein 3264 is independent point (R (int)=0.0892).The equal Jing Lp factors of total data and
Empirical absorption correction.Solved by direct method using SHELXS-97 programs, obtain its structure chart as shown in Fig. 2 its structure and target
Product is consistent.
The above-mentioned metal cobalt complex being prepared into is made into the medicines such as antibacterial tablet, pill, capsule, suspending agent or Emulsion,
And bacteriostatic test is carried out according to GB15979-2002, medicine is played to escherichia coli, staphylococcus aureuses, bacillus subtilises
Very strong bactericidal properties, sterilizing rate reaches more than 95%；Film bacillus is pressed from both sides to aerogenesis and bacillus pyocyaneus play certain bactericidal properties, sterilize
Rate reaches 75-88%.
Embodiment 3
Fig. 1 is the method route schematic diagram that the present invention prepares the metal cobalt complex.With reference to Fig. 1, metallic cobalt of the present invention
The preparation method of coordination compound is comprised the following specific steps that：
1) 1.23g or 10mmol nicotinic acid is placed in into 30ml SOCl2In be heated to reflux stirring 5 hours, be evaporated under reduced pressure solvent,
The nicotinoyl chlorine of white solid is obtained, product is dissolved in without isolation in 30ml chloroforms, add and continue back after 1.22g or 10mmol Isoniazids
Stream 6 hours, is evaporated under reduced pressure gained material ethyl alcohol recrystallization after solvent and obtains 0.78g 3- pyridine radicals -4- pyridine radicals imines；Will
Products therefrom is dissolved in 30ml ethanol solution, sequentially adds 3-4 drops glacial acetic acid and 3ml hydrazine hydrates, under glacial acetic acid catalysis, with
Hydrazine hydrate ring closure reaction, flow back 8h, gained crude product chloroform or recrystallizing methanol after solvent is evaporated under reduced pressure part 3- (4- are obtained
Pyridine radicals) -5- (3- pyridine radicals) -1,2,4- triazoles, the step obtains the total recovery of part and can reach 35%；
2) by the triazoles of 0.15g or 0.55mmol 3- (4- pyridine radicals) -5- (3- pyridine radicals) -1,2,4- and 0.069g or
0.5mmol P-hydroxybenzoic acid is that part and 0.25g or 1mmol cobaltous acetate are placed in heating in autoclave at 120 DEG C and add
Means of press seals is reacted, and has reddish-orange crystals to be formed after 68h, and Jing X- single crystal diffractions are accredited as target product, and the target product is this
Invention metal cobalt complex, chemical name is two (3- (4- pyridine radicals) -5- (3- pyridine radicals) -1,2,4- triazolyls) dihydroxy benzenes
Formic acid closes cobalt (II), and its molecular formula is C38H28CoN10O6, its relative molecular weight is 779.63.
Target product X ray crystal structure is determined below：Choose size and be about 0.40mm × 0.20mm × 0.12mm's
Monocrystalline is placed on the CCD X-ray single crystal diffractometers of Brucker SMART 1000 and carries out diffraction, with Jing graphite monochromator monochromatizations
Mo K alpha raysFor incident wavelength, with ω/2 scan mode in the range of 3.01 ° to 25.24 °
Diffraction data 10129 is collected, wherein 3264 is independent point (R (int)=0.0892).The equal Jing Lp factors of total data and
Empirical absorption correction.Solved by direct method using SHELXS-97 programs, obtain its structure chart as shown in Fig. 2 its structure and target
Product is consistent.
The above-mentioned metal cobalt complex being prepared into is made into antibacterial injection needle, and is carried out according to GB 15979-2002 antibacterial
Test, antibacterial injection needle plays very strong bactericidal properties, sterilizing rate to escherichia coli, staphylococcus aureuses, bacillus subtilises
Reach more than 99%；Film bacillus is pressed from both sides to aerogenesis and bacillus pyocyaneus play certain bactericidal properties, sterilizing rate reaches 80-90%.
Show from the above, metal cobalt complex of the present invention has very strong antibacterial activity, with the metal cobalt complex
The antimicrobial being prepared into has very to harmful bacterias such as escherichia coli, staphylococcus aureuses, bacillus subtilises, bacillus pyocyaneus
Strong bactericidal properties, the present invention provides new thinking to research and develop new antibacterials.
Although embodiment of the present invention is disclosed as above, it is not restricted to listed in description and embodiment
With, it can be applied to completely various suitable the field of the invention, for those skilled in the art, can be easily
Other modification is realized, therefore under the general concept limited without departing substantially from claim and equivalency range, the present invention is not limited
In specific details.
Claims (4)
1. a kind of metal cobalt complex, it is characterised in that：The structural formula of the metal cobalt complex is：
The chemical name of the metal cobalt complex is：Two (3- (4- pyridine radicals) -5- (3- pyridine radicals) -1,2,4- triazolyls) two
Hydroxy benzoic acid closes cobalt (II)；
The molecular formula of the metal cobalt complex is：C38H28CoN10O6；
The relative molecular weight of the metal cobalt complex is：779.63.
2. a kind of method for preparing metal cobalt complex as claimed in claim 1, it is characterised in that methods described includes as follows
Step：
1) by nicotinic acid in SOCl2In be heated to reflux stir 4-5 hour, be evaporated under reduced pressure solvent after obtained by white solid be dissolved in chloroform
In, add Isoniazid after flow back 5-6 hour, be evaporated under reduced pressure solvent after obtained by material ethyl alcohol recrystallization obtain 3- pyridine radicals-
4- pyridine radicals imines, and products therefrom is dissolved in ethanol solution, finally under glacial acetic acid catalysis, and hydrazine hydrate ring closure reaction,
Backflow 8h, is evaporated under reduced pressure gained crude product chloroform or recrystallizing methanol after solvent and obtains part 3- (4- pyridine radicals) -5- (3- pyridines
Base) -1,2,4- triazoles；
2) with 3- (4- pyridine radicals) -5- (3- pyridine radicals) -1,2,4- triazoles and P-hydroxybenzoic acid are that part exists with cobaltous acetate
Capping is carried out at a temperature of 120-200 DEG C, there are reddish-orange crystals to be formed after 48-72h, Jing X- single crystal diffractions are accredited as target
Product.
3. method according to claim 2, it is characterised in that the step 2) capping be in autoclave
Heating pressurization reaction.
4. application of a kind of metal cobalt complex as claimed in claim 1 in antibacterials are prepared.
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| CN201410520605.3A CN104311604B (en) | 2014-09-30 | 2014-09-30 | Metal cobalt compound as well as preparation method and application thereof |
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| CN104311604B true CN104311604B (en) | 2017-05-17 |
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Citations (4)
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| CN103059011A (en) * | 2013-01-22 | 2013-04-24 | 山东师范大学 | Three metal organic frames based on Co(II) ion as well as synthesis method and application thereof |
| CN103724377A (en) * | 2014-01-10 | 2014-04-16 | 中国科学院化学研究所 | 2,6-diene amine pyridine binuclear cobalt complex catalyst as well as preparation method and application thereof |
| CN103804419A (en) * | 2014-03-13 | 2014-05-21 | 山东理工大学 | 2-(4-bromophenyl) quinoline-4-formic acid complex and preparation method and application thereof |
| CN103923126A (en) * | 2014-03-26 | 2014-07-16 | 合肥学院 | Dikaryotic cobalt complex and preparation method thereof |
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| CN103059011A (en) * | 2013-01-22 | 2013-04-24 | 山东师范大学 | Three metal organic frames based on Co(II) ion as well as synthesis method and application thereof |
| CN103724377A (en) * | 2014-01-10 | 2014-04-16 | 中国科学院化学研究所 | 2,6-diene amine pyridine binuclear cobalt complex catalyst as well as preparation method and application thereof |
| CN103804419A (en) * | 2014-03-13 | 2014-05-21 | 山东理工大学 | 2-(4-bromophenyl) quinoline-4-formic acid complex and preparation method and application thereof |
| CN103923126A (en) * | 2014-03-26 | 2014-07-16 | 合肥学院 | Dikaryotic cobalt complex and preparation method thereof |
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