CN103450095A - Mercuric sulfamonomethoxine and preparation method thereof - Google Patents
Mercuric sulfamonomethoxine and preparation method thereof Download PDFInfo
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- CN103450095A CN103450095A CN2013104097919A CN201310409791A CN103450095A CN 103450095 A CN103450095 A CN 103450095A CN 2013104097919 A CN2013104097919 A CN 2013104097919A CN 201310409791 A CN201310409791 A CN 201310409791A CN 103450095 A CN103450095 A CN 103450095A
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Abstract
The invention belongs to sulfonamide transition metal compounds and preparation methods thereof, and specifically relates to mercuric sulfamonomethoxine and a preparation method thereof. The invention mainly solves the technical problem that sulfonamide medicines are poor in antibacterial activity. The technical scheme adopted by the invention is as follows: mercuric sulfamonomethoxine is prepared by synthesizing sulfamonomethoxine and mercuric chloride in ratio of amount of substance of: 2:1. The preparation method comprises the following steps: (1) weighing raw materials according to the ratio of amount of substance of: 2:1 of sulfamonomethoxine toand mercuric chloride; (2) sequentially adding NaOH liquor and sulfamonomethoxine into a container according to the mass ratio of sulfamonomethoxine toand 10% NaOH liquor of (2.9-5.6):10, and stirring to react for 5 hours at normal temperature; (3) preparingproportioning mercuric chloride into 0.255mol/L<-1> mercuric chloride aqueous liquor; (4) adding the mercuric chloride aqueous liquor into the container at 60 DEG C, and insulating to react for 5 hours to generate a mercuric sulfamonomethoxine wet product; (5) decompressing and filtering the produced wet product, washing the product with redistilled water and absolute ethyl alcohol, and vacuum-drying the product at 40 DEG C for 12 hours to obtain the mercuric sulfamonomethoxine product.
Description
Technical field
The invention belongs to sulfamido transition metal complex and preparation method thereof, be specifically related to a kind of sulfamonomethoxine mercury and preparation method thereof.
Background technology
Sulfamonomethoxine is a kind of of sulfa drugs, and it has the obstruction effect to folic acid in bacterial body is synthetic, thereby reaches antibacterial effect, belongs to the sulfamido bacteriostatic.But bacterium increases the sulfa drugs resistance in recent years, as in treatment scald and burn, sulfa drugs can not effectively stop the infection of bacterium in scald and burn.
Summary of the invention
The objective of the invention is to solve the sulfa drugs technical problem poor to the biocidal property of bacterium, a kind of sulfamonomethoxine mercury and preparation method thereof is provided, the present invention has good biocidal property to intestinal bacteria, streptococcus aureus, Bacillus subtilus, and the preparation method is simple, with low cost, be easy to industrialization.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
A kind of sulfamonomethoxine mercury, it is with mercury chloride, by the amount of substance ratio, to be that the 2:1 chemosynthesis makes by sulfamonomethoxine, the structural formula of sulfamonomethoxine mercury is:
Molecular formula is: C
22h
22n
8o
6s
2hg.
The preparation method of above-mentioned sulfamonomethoxine mercury, its preparation process is: 1. according to sulfamonomethoxine and mercury chloride amount of substance ratio, for 2:1, take each raw material; The NaOH solution that the proportioning that the mass ratio of the NaOH solution that is 2. 10% according to sulfamonomethoxine and concentration is 2.9～5.6:10 is 10% by concentration is put into reaction vessel, then sulfamonomethoxine is added in container, and magnetic agitation is reacted 5h at normal temperatures; 3. mercury chloride is dissolved in redistilled water to be made into concentration be 0.255molL
-1mercuric chloride solution; 4. reaction vessel is placed in to the temperature of 60 ℃, continues to stir, mercuric chloride solution is slowly at the uniform velocity added in reaction vessel, insulation reaction 5h, generate a large amount of pale precipitations and be sulfamonomethoxine mercury wet product; 5. sulfamonomethoxine mercury wet product filtration under diminished pressure reaction generated, use the second distillation water washing, then use absolute ethanol washing, and 40 ℃ of vacuum-drying 12h obtain sulfamonomethoxine mercury product.
For showing the bacteriostasis property of the present invention to intestinal bacteria, streptococcus aureus, Bacillus subtilus, adopt the In Vitro Bacteriostasis test.
1. medicine and bacterial strain
The self-control of sulfamonomethoxine mercury, Gram-negative bacteria, gram-positive microorganism all are purchased from Qingdao GaoKeYuan Hai Bo Bioisystech Co., Ltd.
2. method
The microbial culture plate is put 37 ℃ and is cultivated 24h, and 28 ℃ of cultivation 24h of fungi, adopt nutrient broth By Dilution SMD, HgCl
2and the minimum inhibitory concentration of SMD-Hg (II), observations, data see the following form 1.
Table 1SMD, HgCl
2and the minimum inhibitory concentration (MIC) of SMD-Hg (II)/mgmL
-1
From minimum inhibitory concentration, bacterium class title complex minimum inhibitory concentration all is less than part, show that title complex is better than part to each bacterial classification bacteriostasis property, illustrate that the sulfamonomethoxine hydrargyrum complex has good biocidal property to intestinal bacteria, streptococcus aureus, Bacillus subtilus.
Embodiment
Embodiment 1
Sulfamonomethoxine mercury in the present embodiment, it is with mercury chloride, by the amount of substance ratio, to be that the 2:1 chemosynthesis makes by sulfamonomethoxine, the structural formula of sulfamonomethoxine mercury is:
Molecular formula is: C
22h
22n
8o
6s
2hg.
The preparation method of above-mentioned sulfamonomethoxine mercury, its preparation process is: 1. take raw material sulfamonomethoxine 2.90g and mercury chloride 1.40g; 2. the NaOH solution that is 10% by 10g concentration is put into reaction vessel, then the 2.90g sulfamonomethoxine is added in container, and magnetic agitation is reacted 5h at normal temperatures; 3. 1.40g mercury chloride is dissolved in redistilled water to be made into concentration be 0.255molL
-1mercuric chloride solution; 4. reaction vessel is placed in to the water-bath of 60 ℃, continues to stir, mercuric chloride solution is slowly at the uniform velocity added in reaction vessel, insulation reaction 5h, generate a large amount of pale precipitations and be sulfamonomethoxine mercury wet product; 5. sulfamonomethoxine mercury wet product filtration under diminished pressure reaction generated, use the second distillation water washing, then use absolute ethanol washing, and 40 ℃ of vacuum-drying 12h, obtain sulfamonomethoxine mercury product 2.51g, productive rate 66.15%.
Embodiment 2
Sulfamonomethoxine mercury in the present embodiment is identical with the sulfamonomethoxine mercury in embodiment 1.
The preparation method of above-mentioned sulfamonomethoxine mercury, its preparation process is: 1. take raw material sulfamonomethoxine 3.48g and mercury chloride 1.69g; 2. the NaOH solution that is 10% by 10g concentration is put into reaction vessel, then the 3.48g sulfamonomethoxine is added in container, and magnetic agitation is reacted 5h at normal temperatures; 3. 1.69g mercury chloride is dissolved in redistilled water to be made into concentration be 0.255molL
-1mercuric chloride solution; 4. reaction vessel is placed in to the water-bath of 60 ℃, continues to stir, mercuric chloride solution is slowly at the uniform velocity added in reaction vessel, insulation reaction 5h, generate a large amount of pale precipitations and be sulfamonomethoxine mercury wet product; 5. sulfamonomethoxine mercury wet product filtration under diminished pressure reaction generated, use the second distillation water washing, then use absolute ethanol washing, and 40 ℃ of vacuum-drying 12h, obtain sulfamonomethoxine mercury product 3.15g, productive rate 69.97%.
Embodiment 3
Sulfamonomethoxine mercury in the present embodiment is identical with the sulfamonomethoxine mercury in embodiment 1.
The preparation method of above-mentioned sulfamonomethoxine mercury, its preparation process is: 1. take raw material sulfamonomethoxine 4.26g and mercury chloride 2.06g; 2. the NaOH solution that is 10% by 10g concentration is put into reaction vessel, then the 4.26g sulfamonomethoxine is added in container, and magnetic agitation is reacted 5h under normal temperature environment; 3. 2.06g mercury chloride is dissolved in redistilled water to be made into concentration be 0.255molL
-1mercuric chloride solution; 4. reaction vessel is placed in to the water-bath of 60 ℃, continues to stir, mercuric chloride solution is slowly at the uniform velocity added in reaction vessel, insulation reaction 5h, generate a large amount of pale precipitations and be sulfamonomethoxine mercury wet product; 5. sulfamonomethoxine mercury wet product filtration under diminished pressure reaction generated, use the second distillation water washing, then use absolute ethanol washing, and 40 ℃ of vacuum-drying 12h, obtain sulfamonomethoxine mercury product 3.15g, productive rate 55.42%.
Embodiment 4
Sulfamonomethoxine mercury in the present embodiment is identical with the sulfamonomethoxine mercury in embodiment 1.
The preparation method of above-mentioned sulfamonomethoxine mercury, its preparation process is: 1. take raw material sulfamonomethoxine 5.60g and mercury chloride 2.70g; 2. the NaOH solution that is 10% by 10g concentration is put into reaction vessel, then the 5.60g sulfamonomethoxine is added in container, and magnetic agitation is reacted 5h under normal temperature environment; 3. 2.70g mercury chloride is dissolved in redistilled water to be made into concentration be 0.255molL
-1mercuric chloride solution; 4. reaction vessel is placed in to the temperature of 60 ℃, continues to stir, mercuric chloride solution is slowly at the uniform velocity added in reaction vessel, insulation reaction 5h, generate a large amount of pale precipitations and be sulfamonomethoxine mercury wet product; 5. sulfamonomethoxine mercury wet product filtration under diminished pressure reaction generated, use the second distillation water washing, then use absolute ethanol washing, and 40 ℃ of vacuum-drying 12h, obtain sulfamonomethoxine mercury product 7.10g, productive rate 93.66%.
Protection scope of the present invention is not subject to the restriction of above embodiment.
Claims (2)
1. a sulfamonomethoxine mercury, it is characterized in that: it is with mercury chloride, by the amount of substance ratio, to be that the 2:1 chemosynthesis makes by sulfamonomethoxine, and the structural formula of sulfamonomethoxine mercury is:
Molecular formula is: C
22h
22n
8o
6s
2hg.
2. the preparation method of a sulfamonomethoxine mercury, is characterized in that: 1. according to sulfamonomethoxine and mercury chloride amount of substance ratio, for 2:1, take each raw material; The NaOH solution that the proportioning that the mass ratio of the NaOH solution that is 2. 10% according to sulfamonomethoxine and concentration is 2.9～5.6:10 is 10% by concentration is put into reaction vessel, then sulfamonomethoxine is added in container, and magnetic agitation is reacted 5h at normal temperatures; 3. mercury chloride is dissolved in redistilled water to be made into concentration be 0.255molL
-1mercuric chloride solution; 4. reaction vessel is placed in to the temperature of 60 ℃, continues to stir, mercuric chloride solution is slowly at the uniform velocity added in reaction vessel, insulation reaction 5h, generate a large amount of pale precipitations and be sulfamonomethoxine mercury wet product; 5. sulfamonomethoxine mercury wet product filtration under diminished pressure reaction generated, use the second distillation water washing, then use absolute ethanol washing, and 40 ℃ of vacuum-drying 12h obtain sulfamonomethoxine mercury product.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111606933A (en) * | 2020-06-30 | 2020-09-01 | 洛阳师范学院 | Phenanthroline ligand-containing Cd (II) complex and preparation method and application thereof |
| CN112079852A (en) * | 2020-08-21 | 2020-12-15 | 洛阳师范学院 | Zn (II) complex based on ASBSA and 4, 4' bipyridyl ligand and preparation method and application thereof |
| CN114716388A (en) * | 2021-11-04 | 2022-07-08 | 江苏冠军科技集团股份有限公司 | Sulfanilamide-silver compound and preparation method thereof |
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| CN103006674A (en) * | 2012-12-14 | 2013-04-03 | 江苏恒丰强生物技术有限公司 | Compound sulfamonomethoxine sodium solution and preparation method thereof |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103006674A (en) * | 2012-12-14 | 2013-04-03 | 江苏恒丰强生物技术有限公司 | Compound sulfamonomethoxine sodium solution and preparation method thereof |
Non-Patent Citations (4)
| Title |
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| ANGEL GARCIA-RASO,ETAL: "Coordination behaviour of sulfanilamide derivatives. Crystal structures of [Hg(sulfamethoxypyridazinato)2], [Cd(sulfadimidinato)2(H2O)] 2H2O and[Zn(sulfamethoxazolato)2-(pyridine)2(H2O)2]", 《POLYHEDRON》, no. 19, 31 December 2000 (2000-12-31), pages 991 - 1004 * |
| ANGEL GARCIA-RASO,ETAL: "Metallation of 2-sulfanilamidopyrimidine (sulfadiazine).X-ray diffraction structure and solution behaviour of bis(sulfadiazinato) mercury bis(dimethylsulfoxide)", 《POLYHEDRON》, vol. 16, no. 4, 31 December 1997 (1997-12-31), pages 613 - 621, XP005504685, DOI: doi:10.1016/0277-5387(96)00317-8 * |
| G.M.GOLZAR HOSSAIN,ETAL: "Syntheses and characterisation of mercury complexes of sulfadiazine, sulfamerazine and sulfamethazine", 《POLYHEDRON》, no. 26, 31 December 2007 (2007-12-31), pages 967 - 974 * |
| 尹爱萍: "磺胺间甲氧嘧啶过渡金属配合物的制备及其表征", 《内蒙古石油化工》, no. 18, 30 September 2011 (2011-09-30), pages 4 - 6 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111606933A (en) * | 2020-06-30 | 2020-09-01 | 洛阳师范学院 | Phenanthroline ligand-containing Cd (II) complex and preparation method and application thereof |
| CN112079852A (en) * | 2020-08-21 | 2020-12-15 | 洛阳师范学院 | Zn (II) complex based on ASBSA and 4, 4' bipyridyl ligand and preparation method and application thereof |
| CN112079852B (en) * | 2020-08-21 | 2023-01-10 | 洛阳师范学院 | Zn (II) complex based on ASBSA and 4,4' bipyridine ligand and preparation method and application thereof |
| CN114716388A (en) * | 2021-11-04 | 2022-07-08 | 江苏冠军科技集团股份有限公司 | Sulfanilamide-silver compound and preparation method thereof |
| CN114716388B (en) * | 2021-11-04 | 2024-02-13 | 江苏冠军科技集团股份有限公司 | Sulfonamide-silver compound and preparation method thereof |
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Application publication date: 20131218 |