CN103467499A - Copper complex with 2,2'-dipyridyl and preparation method thereof - Google Patents
Copper complex with 2,2'-dipyridyl and preparation method thereof Download PDFInfo
- Publication number
- CN103467499A CN103467499A CN 201310424590 CN201310424590A CN103467499A CN 103467499 A CN103467499 A CN 103467499A CN 201310424590 CN201310424590 CN 201310424590 CN 201310424590 A CN201310424590 A CN 201310424590A CN 103467499 A CN103467499 A CN 103467499A
- Authority
- CN
- China
- Prior art keywords
- dipyridyl
- copper complex
- preparation
- bipyridine
- pyridine
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical group N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 150000004699 copper complex Chemical class 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000010949 copper Substances 0.000 claims abstract description 20
- JUJWROOIHBZHMG-UHFFFAOYSA-N pyridine Substances C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000126 substance Substances 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 4
- 239000010935 stainless steel Substances 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000013078 crystal Substances 0.000 claims description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 2
- XVMSFILGAMDHEY-UHFFFAOYSA-N 6-(4-aminophenyl)sulfonylpyridin-3-amine Chemical compound C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=N1 XVMSFILGAMDHEY-UHFFFAOYSA-N 0.000 claims 1
- 238000001027 hydrothermal synthesis Methods 0.000 claims 1
- 150000003891 oxalate salts Chemical class 0.000 claims 1
- 239000000047 product Substances 0.000 claims 1
- 238000001338 self-assembly Methods 0.000 claims 1
- 125000006850 spacer group Chemical group 0.000 claims 1
- -1 polytetrafluoroethylene Polymers 0.000 abstract description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 abstract description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 abstract description 3
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 abstract description 3
- 238000012546 transfer Methods 0.000 abstract description 2
- 229910052802 copper Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 239000003814 drug Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003446 ligand Substances 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000001093 anti-cancer Effects 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001879 copper Chemical class 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000002447 crystallographic data Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000005232 molecular self-assembly Methods 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000013268 sustained release Methods 0.000 description 1
- 239000012730 sustained-release form Substances 0.000 description 1
Images
Landscapes
- Pyridine Compounds (AREA)
Abstract
本发明涉及一种带有2，2’-联吡啶的铜配合物及其制备方法。它是下述化学式(I)的配合物，[Cu(L)(C2O4)]·H2O，其中L＝2，2’-联吡啶；它具有一维的链状空间结构。将Cu(CH3COO)2·H2O、2，3，5-吡啶三酸和2，2’-联吡啶溶于10mL水中，滴加一滴吡啶，然后将溶液移入有聚四氟乙烯内衬的不锈钢反应釜中密封，110℃反应三天，降到室温。溶液过滤、静置、挥发，得到目标产品。The invention relates to a copper complex with 2,2'-bipyridine and a preparation method thereof. It is a complex of the following chemical formula (I), [Cu(L)(C 2 O 4 )]·H 2 O, wherein L=2,2'-bipyridine; it has a one-dimensional chain space structure. Dissolve Cu(CH 3 COO) 2 ·H 2 O, 2,3,5-pyridine triacid and 2,2'-bipyridine in 10mL of water, add a drop of pyridine, and then transfer the solution into polytetrafluoroethylene Seal it in a lined stainless steel reaction kettle, react at 110°C for three days, and cool down to room temperature. The solution was filtered, allowed to stand, and volatilized to obtain the target product.
Description
技术领域technical field
本发明属于配合物科学与技术领域，特别涉及带有2，2’-联吡啶的铜配合物的制备方法。The invention belongs to the field of complex science and technology, in particular to a preparation method of a copper complex with 2,2'-bipyridine.
技术背景technical background
近年来，金属有机配合物的合成制备得到科学界的广泛关注，它们在气体存储，选择性分离，催化，药物缓释等领域具有潜在的应用价值。铜金属配合物的合成在诸多的金属配合物占重要作用。在医学领域，铜的金属配合物具有抗肿瘤活性，成为无机抗癌配合物研究的重点[李雪等，广东化工，108 39 2012]；在应用化学领域，铜配合物晶体可以作为液晶材料，是液晶材料研究的重点[赵鸿斌等 化学学报331 64 2006]。金属铜的配合物中，配体的种类、配合物的空间结构等因素对其物理化学性质都会产生不同的影响。因此，通过配体调控以及分子自组装，设计合成具有新颖空间结构以及功能的铜配合物是各国科学家追求的共同目标。In recent years, the synthesis and preparation of metal-organic complexes has attracted widespread attention in the scientific community, and they have potential applications in the fields of gas storage, selective separation, catalysis, and sustained release of drugs. The synthesis of copper metal complexes plays an important role in many metal complexes. In the field of medicine, copper metal complexes have anti-tumor activity and become the focus of research on inorganic anti-cancer complexes [Li Xue et al., Guangdong Chemical Industry, 108 39 2012]; in the field of applied chemistry, copper complex crystals can be used as liquid crystal materials, It is the focus of research on liquid crystal materials [Zhao Hongbin et al., Acta Chem. Sinica 331 64 2006]. In the complexes of metal copper, factors such as the type of ligands and the spatial structure of the complexes will have different effects on their physical and chemical properties. Therefore, it is a common goal pursued by scientists from all over the world to design and synthesize copper complexes with novel spatial structures and functions through ligand regulation and molecular self-assembly.
发明内容Contents of the invention
本发明的目的是提供一种含2，2’-联吡啶的铜配合物的制备方法。该金属铜配合物具有一维链状空间结构，具有广泛的应用前景。The purpose of this invention is to provide a kind of preparation method containing the copper complex of 2,2'-bipyridine. The metal copper complex has a one-dimensional chain space structure and has broad application prospects.
本发明提供的铜配合物的化学式为[Cu(L)(C2O4)]·H2O，其中L＝2，2’-联吡啶。The chemical formula of the copper complex provided by the present invention is [Cu(L)(C 2 O 4 )]·H 2 O, wherein L=2,2'-bipyridine.
本发明公开的铜配合物的结构如图1所示，它们的二级结构单元为：晶体属于三斜晶系，空间群为P-1，晶胞参数为：α＝111.188(3)°，β＝97.329(4)°，γ＝104.965(4)°；该配合物的空间结构是以铜原子为中心，2，2’-联吡啶和草酸根离子自组装而形成的一维链状结构；Cu离子的配位数是6，与来自一个2，2’-联吡啶中的两个N原子和来自两个草酸根中的四个O原子配位；它们以Cu为中心形成扭曲的八面体。N1、N2、O1、O3处在八面体的赤道面上，它们对应的键长和夹角分别为：Cu1-N1，
本发明的制备方法如下：The preparation method of the present invention is as follows:
将Cu(CH3COO)2·H2O、2，3，5-吡啶三酸和2，2’-联吡啶溶于10ml水中，滴加一滴吡啶，然后将溶液移入有聚四氟乙烯内衬的不锈钢反应釜中密封，保持温度为110℃三天，然后以每小时5℃的速度降低温度到室温。将溶液过滤，滤液室温下静置，大约一周后可得到蓝色结晶。Cu(CH3COO)2·H2O、2，3，5-吡啶三酸、2，2’-联吡啶的质量之比为1.92∶1.35∶1。Dissolve Cu(CH 3 COO) 2 ·H 2 O, 2,3,5-pyridine triacid and 2,2'-bipyridine in 10ml of water, add a drop of pyridine, and then transfer the solution into polytetrafluoroethylene The lined stainless steel reactor was sealed, and the temperature was kept at 110°C for three days, and then the temperature was lowered to room temperature at a rate of 5°C per hour. The solution was filtered, and the filtrate was allowed to stand at room temperature, and blue crystals could be obtained after about a week. The mass ratio of Cu(CH 3 COO) 2 ·H 2 O, 2,3,5-pyridine triacid, and 2,2'-bipyridyl was 1.92:1.35:1.
附图说明Description of drawings
图1[Cu(L)(C2O4)]·H2O的晶体结构图；Fig. 1 Crystal structure diagram of [Cu(L)(C 2 O 4 )]·H 2 O;
图2化合物的一维链状结构图。Figure 2 One-dimensional chain structure diagram of the compound.
表1配合物的晶体学数据Crystallographic data of the complexes in Table 1
具体实施方式Detailed ways
实施例1配合物的合成：The synthesis of embodiment 1 complex:
将0.15mmol的Cu(CH3COO)2·H2O(0.030g)、0.1mmol的2，3，5-吡啶三酸(0.0212g)和0.1mmol的2，2’-联吡啶(0.0156g)溶于10ml水中，滴加一滴吡啶，然后把溶液移入15mL的有聚四氟乙烯内衬的不锈钢反应釜中密封，保持温度为110℃三天，然后以每小时5℃的速度降低温度到室温。将溶液过滤，滤液室温下静置，大约一周后可得到蓝色结晶。基于金属铜计算产率为30％。0.15mmol of Cu(CH 3 COO) 2 ·H 2 O (0.030g), 0.1mmol of 2,3,5-pyridine triacid (0.0212g) and 0.1mmol of 2,2'-bipyridine (0.0156g ) was dissolved in 10ml of water, a drop of pyridine was added dropwise, and then the solution was transferred into a 15mL stainless steel reaction kettle lined with polytetrafluoroethylene and sealed. The temperature was kept at 110°C for three days, and then the temperature was lowered to room temperature. The solution was filtered, and the filtrate was allowed to stand at room temperature, and blue crystals could be obtained after about a week. The yield was calculated to be 30% based on metallic copper.
实施例2配合物的结构测定：The structural determination of embodiment 2 complexes:
晶体结构测定采用BRUKER SMART1000X-射线衍射仪，使用经过石墨单色化的Mokα射线(
Claims (5)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201310424590 CN103467499A (en) | 2013-09-13 | 2013-09-13 | Copper complex with 2,2'-dipyridyl and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201310424590 CN103467499A (en) | 2013-09-13 | 2013-09-13 | Copper complex with 2,2'-dipyridyl and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103467499A true CN103467499A (en) | 2013-12-25 |
Family
ID=49792569
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201310424590 Pending CN103467499A (en) | 2013-09-13 | 2013-09-13 | Copper complex with 2,2'-dipyridyl and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103467499A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103864823A (en) * | 2014-03-14 | 2014-06-18 | 洛阳师范学院 | Cu (I) coordination polymer green light emitting material and synthesis method thereof |
| CN105646549A (en) * | 2016-01-13 | 2016-06-08 | 山西大学 | Double-terminal-group pyridine copper complex and preparation method thereof |
| CN106397786A (en) * | 2016-09-12 | 2017-02-15 | 广西师范大学 | 3-carboxyl-5-thioketone-1,2,4-triazole copper coordination polymer and in-situ synthesis method thereof |
-
2013
- 2013-09-13 CN CN 201310424590 patent/CN103467499A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103864823A (en) * | 2014-03-14 | 2014-06-18 | 洛阳师范学院 | Cu (I) coordination polymer green light emitting material and synthesis method thereof |
| CN103864823B (en) * | 2014-03-14 | 2016-08-24 | 洛阳师范学院 | A kind of Cu (I) coordination polymer green luminescent material and synthetic method thereof |
| CN105646549A (en) * | 2016-01-13 | 2016-06-08 | 山西大学 | Double-terminal-group pyridine copper complex and preparation method thereof |
| CN106397786A (en) * | 2016-09-12 | 2017-02-15 | 广西师范大学 | 3-carboxyl-5-thioketone-1,2,4-triazole copper coordination polymer and in-situ synthesis method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103772418B (en) | A kind of ligand polymer with mixed ligand and preparation method thereof | |
| CN102993222B (en) | Dysprosium coordination polymer material with solvent molecule magnetic response and preparation method thereof | |
| Xu et al. | Two 2D→ 3D entangled coordination polymers with polycatenated and polythreaded features based on 4 4-sql layers | |
| Semerci et al. | Self-assembly of three new metal organic coordination networks based on 1, 2-bis (imidazol-1yl-methyl) benzene | |
| CN103467499A (en) | Copper complex with 2,2'-dipyridyl and preparation method thereof | |
| Huang et al. | Two novel interpenetrating MOFs constructed from a derivative of phenanthroline and a V-shaped flexible dicarboxylate ligand contains unique chiral structure | |
| CN105001246A (en) | 8-aminoquinoline Schiff base zinc azide metal complex and preparation method thereof | |
| Zheng et al. | Structures and properties of five main group coordination polymers based on 2-(pyridin-4-yl)-1H-imidazole-4, 5-dicarboxylate | |
| Chen et al. | Syntheses, structures and thermal properties of two new copper (II) melamine complexes | |
| CN105669774B (en) | A kind of linear five core Ln of zero dimension2Co3Magnetic material and preparation method thereof | |
| CN104292247B (en) | A kind of have mixed ligand containing cadmium two-dimensional polymer and preparation method thereof | |
| CN105646549A (en) | Double-terminal-group pyridine copper complex and preparation method thereof | |
| CN102977128B (en) | Metal-free radical complex type magnetic material, as well as preparation and application thereof | |
| Yang et al. | A new mixed-ligand copper pentaborate with square-like, rectangle-like and ellipse-like channels formed via hydrogen bonds | |
| Li et al. | Solvent-controlled formation of four Ni (II) coordination polymers based on a flexible bis (imidazole) ligand: syntheses, structural diversification, properties | |
| CN104341440B (en) | 4-tert-butyl o phthalic acid Zn complex and preparation method thereof | |
| CN102702239A (en) | Transitional cadmium metal coordination compound with pyrazine tricarboxylic acid as organic ligand and preparation method of coordination compound | |
| CN106543142A (en) | A kind of complex of (3 (3 yl of pyridine) 1,2,4 triazoles of 1H, 5 yl) benzoic acid cadmium and preparation method thereof | |
| Zhou et al. | Syntheses, structures and properties of metal-carboxylate chain-based coordination polymers (CPs) with 1, 1′: 4′, 1 ″-terphenyl-2′, 4, 4 ″, 5′-tetracarboxylate | |
| CN108424429B (en) | Three-dimensional porous structure of Cd(II) and K(I) complexes and their preparation methods and applications | |
| CN104130292A (en) | Three dimensional coordination polymer with double core structure and preparation method thereof | |
| CN109021031A (en) | 5- bromopyridine -2,3- dicarboxylic acids nickel complex and preparation method thereof | |
| Li et al. | Four homochiral coordination polymers contain N-acetyl-L-tyrosine and different N-donor ligand: Influence of metal cations, ancillary ligands and coordination modes | |
| Hu et al. | Time-of-diffusion dependent structural diversity in the MII-phen-tetracyanometalates (M= Zn, Mn) supramolecular system | |
| Xiao et al. | Synthesis, crystal structure and optical property of two zinc metal organic frameworks constructed from isonicotinic acid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20131225 |
|
| WD01 | Invention patent application deemed withdrawn after publication |