CN107266506A - A kind of cobalt nitrouracil super molecular compound and preparation method thereof - Google Patents
A kind of cobalt nitrouracil super molecular compound and preparation method thereof Download PDFInfo
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- CN107266506A CN107266506A CN201710439529.7A CN201710439529A CN107266506A CN 107266506 A CN107266506 A CN 107266506A CN 201710439529 A CN201710439529 A CN 201710439529A CN 107266506 A CN107266506 A CN 107266506A
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- cobalt
- molecular compound
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- 150000001875 compounds Chemical class 0.000 title claims abstract description 38
- FJMGHHNXDDNEJN-UHFFFAOYSA-N [N+](=O)([O-])C=1C(NC(NC1)=O)=O.[Co] Chemical compound [N+](=O)([O-])C=1C(NC(NC1)=O)=O.[Co] FJMGHHNXDDNEJN-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical compound N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 239000000126 substance Substances 0.000 claims abstract description 12
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910001429 cobalt ion Inorganic materials 0.000 claims abstract description 8
- 230000036571 hydration Effects 0.000 claims description 14
- 238000006703 hydration reaction Methods 0.000 claims description 14
- 239000013078 crystal Substances 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000011541 reaction mixture Substances 0.000 claims description 7
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- CXHLVSRLJAYJLY-UHFFFAOYSA-N O.[K].[N+](=O)([O-])C1=C(C(=O)O)NC(NC1=O)=O Chemical class O.[K].[N+](=O)([O-])C1=C(C(=O)O)NC(NC1=O)=O CXHLVSRLJAYJLY-UHFFFAOYSA-N 0.000 claims description 5
- 238000007605 air drying Methods 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 229940011182 cobalt acetate Drugs 0.000 claims description 4
- 210000002700 urine Anatomy 0.000 claims description 3
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims 2
- IFOZXUMSHBVSMA-UHFFFAOYSA-N 5-nitro-2,4-dioxo-1h-pyrimidine-6-carboxylic acid;potassium Chemical compound [K].OC(=O)C=1NC(=O)NC(=O)C=1[N+]([O-])=O IFOZXUMSHBVSMA-UHFFFAOYSA-N 0.000 claims 1
- 206010015856 Extrasystoles Diseases 0.000 claims 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 claims 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims 1
- RDRCCJPEJDWSRJ-UHFFFAOYSA-N pyridine;1h-pyrrole Chemical compound C=1C=CNC=1.C1=CC=NC=C1 RDRCCJPEJDWSRJ-UHFFFAOYSA-N 0.000 claims 1
- 150000002500 ions Chemical class 0.000 abstract description 7
- 238000010276 construction Methods 0.000 abstract description 6
- 229910017052 cobalt Inorganic materials 0.000 abstract description 5
- 239000010941 cobalt Substances 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 abstract description 4
- WJFDCFHWFHCLIW-UHFFFAOYSA-N 2-(bromomethyl)-6-methylpyridine Chemical compound CC1=CC=CC(CBr)=N1 WJFDCFHWFHCLIW-UHFFFAOYSA-N 0.000 abstract 1
- 150000001869 cobalt compounds Chemical class 0.000 abstract 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 229910052700 potassium Inorganic materials 0.000 abstract 1
- 239000011591 potassium Substances 0.000 abstract 1
- 229910052739 hydrogen Inorganic materials 0.000 description 7
- 239000001257 hydrogen Substances 0.000 description 7
- 238000000034 method Methods 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000001338 self-assembly Methods 0.000 description 4
- OPGJGRWULGFTOS-UHFFFAOYSA-N 5-nitro-2,4-dioxo-1h-pyrimidine-6-carboxylic acid Chemical compound OC(=O)C=1NC(=O)NC(=O)C=1[N+]([O-])=O OPGJGRWULGFTOS-UHFFFAOYSA-N 0.000 description 3
- 239000005862 Whey Substances 0.000 description 3
- 102000007544 Whey Proteins Human genes 0.000 description 3
- 108010046377 Whey Proteins Proteins 0.000 description 3
- 238000009825 accumulation Methods 0.000 description 3
- 150000004032 porphyrins Chemical class 0.000 description 3
- LTUDISCZKZHRMJ-UHFFFAOYSA-N potassium;hydrate Chemical compound O.[K] LTUDISCZKZHRMJ-UHFFFAOYSA-N 0.000 description 3
- ZTGWXXOUUKHQLW-UHFFFAOYSA-N 1-nitropyrimidine-2,4-dione Chemical compound [O-][N+](=O)N1C=CC(=O)NC1=O ZTGWXXOUUKHQLW-UHFFFAOYSA-N 0.000 description 2
- 239000005725 8-Hydroxyquinoline Substances 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 2
- CZPWVGJYEJSRLH-UHFFFAOYSA-N Pyrimidine Chemical compound C1=CN=CN=C1 CZPWVGJYEJSRLH-UHFFFAOYSA-N 0.000 description 2
- ISAKRJDGNUQOIC-UHFFFAOYSA-N Uracil Chemical compound O=C1C=CNC(=O)N1 ISAKRJDGNUQOIC-UHFFFAOYSA-N 0.000 description 2
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- UJMDYLWCYJJYMO-UHFFFAOYSA-N benzene-1,2,3-tricarboxylic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1C(O)=O UJMDYLWCYJJYMO-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000001142 circular dichroism spectrum Methods 0.000 description 2
- 150000003983 crown ethers Chemical class 0.000 description 2
- 230000009881 electrostatic interaction Effects 0.000 description 2
- 150000004676 glycans Chemical class 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 230000009878 intermolecular interaction Effects 0.000 description 2
- 239000003446 ligand Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229960003540 oxyquinoline Drugs 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- MCJGNVYPOGVAJF-UHFFFAOYSA-N quinolin-8-ol Chemical compound C1=CN=C2C(O)=CC=CC2=C1 MCJGNVYPOGVAJF-UHFFFAOYSA-N 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- HEALSPFCFYXUNT-UHFFFAOYSA-N 4,4-dimethyl-2-pyridin-2-yl-3h-pyridine Chemical class C1=CC(C)(C)CC(C=2N=CC=CC=2)=N1 HEALSPFCFYXUNT-UHFFFAOYSA-N 0.000 description 1
- TUARVSWVPPVUGS-UHFFFAOYSA-N 5-nitrouracil Chemical compound [O-][N+](=O)C1=CNC(=O)NC1=O TUARVSWVPPVUGS-UHFFFAOYSA-N 0.000 description 1
- 108010022579 ATP dependent 26S protease Proteins 0.000 description 1
- PQYJRMFWJJONBO-UHFFFAOYSA-N Tris(2,3-dibromopropyl) phosphate Chemical compound BrCC(Br)COP(=O)(OCC(Br)CBr)OCC(Br)CBr PQYJRMFWJJONBO-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 239000012491 analyte Substances 0.000 description 1
- 230000003466 anti-cipated effect Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005281 excited state Effects 0.000 description 1
- 229940088597 hormone Drugs 0.000 description 1
- 239000005556 hormone Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 150000001455 metallic ions Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229940035893 uracil Drugs 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 Table
- C07F15/06—Cobalt compounds
- C07F15/065—Cobalt compounds without a metal-carbon linkage
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/13—Crystalline forms, e.g. polymorphs
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pyridine Compounds (AREA)
Abstract
The invention discloses a kind of cobalt nitrouracil super molecular compound and preparation method thereof, the super molecular compound is a kind of cobalt compound with exact space structure, and its chemical formula is CoC18H32N8O18, construction unit is [Co (bpy) (H2O)4]·2(C4H2N3O4)·6H2O (bpy=4,4 ' second bipyridines), crystallographic system is anorthic system, and space group is P 1, and cell parameter isα=86.746 °, β=79.405 °, γ=74.842 °, cobalt ions is the octahedra geometric configuration of hexa-coordinate.The preparation method of the cobalt nitrouracil super molecular compound is：5 nitroorotic acid potassium monohydrates, 4,4 ' second bipyridine parts and the cobalt ions with electro-chemical activity are subjected to self-assembling reaction, a kind of cobalt super molecular compound is made.The preparation method is simple to operate, with low cost, is adapted to large-scale production.Cobalt super molecular compound obtained by the present invention has potential application prospect in terms of ion identification, Subjective and Objective molecule (ion) exchange and electrochemical sensing.
Description
Technical field
The invention belongs to supramolecular chemistry field, and in particular to a kind of cobalt nitrouracil super molecular compound and its preparation
Method.
Background technology
Supermolecule has certain knot by two or more secondary units by one formed by intermolecular force
The molecule aggregate of structure and function.Intermolecular force in supermolecule belongs to non-covalent bond, typically electrostatic interaction, hydrogen bond and
Van der Waals force etc..The inclusion compound of supermolecule generally existing, such as enzyme and its substrate, hormone and its acceptor and crown ether and some metals is all
It is supermolecule." supramolecular chemistry " this concept is proposed first in 1978 by French scientist J.M.Lehn, and in 1987
Obtain Nobel chemistry Prize.He points out:" molecular chemistry field is had based on covalent bond, based on molecular assembly and intermolecular
Key and there is supramolecular chemistry ".Supramolecular chemistry is gathered based on molecule formed by intermolecular non-covalent interaction
The chemistry of collective, in other words intermolecular interaction is the core of supramolecular chemistry.In supramolecular chemistry, different type
Intermolecular interaction can distinguish, according to their different degree of strength, be orientated and adjust the distance with angle according to
Rely degree, can be divided into：Coordinate bond, hydrogen bond, pi-pi accumulation effect, electrostatic interaction and hydrophobic effect of metal ion etc..They
Intensity distribution is by pi-pi accumulation effect and weak to medium, to the strong of metallic ion coordination key or very strong, these active forces of hydrogen bond
Basic skills as driving Supramolecular self assembly.People can be according to Supramolecular self assembly principle, using intermolecular mutual
Active force is assembled into component or building block with specific 26S Proteasome Structure and Function according to certain mode new as instrument
Super molecular compound.These new compounds are not only only capable of showing the special property not available for individual molecule, moreover it is possible to significantly
Increase the species and number of compound.If people can be good at controlling Supramolecular self assembly process, it is possible to it is anticipated that
Simpler, the more reliable compound obtained with specific structure and function of target.
Research finds that 4,4- dimethylbipyridines can be well matched with into the hole of porphyrin and crown ether formation, in illumination
Under the conditions of, the porphyrin excited state molecule of generation can carry out electro transfer well, form a good photoswitch model,
There is potential application in photochemistry.The Subjective and Objective adaptation principle of supramolecular chemistry, is obtained extensively in piezoelectric chemical sensor
Application.Supermolecule is used as the sensitive coating of piezoelectric chemical sensor, using the special space structure of supermolecule, by intermolecular
Synergy, to target molecule carry out molecular recognition.The analyte for meeting space structure is selectively adsorbed, can be obvious
Improve the selectivity of piezoelectric chemical sensor.Supermolecule main block (or acceptor) is to object (or substrate) selective binding and produces certain
The process of specific function is planted, makes its super molecular compound that there is specific identification.It is that part can be closed using benzenetricarboxylic acid (TMA)
Into [Cu3(TMA)(H2O)3]nCoordination supramolecule crystal, makes to manufacture nano level Porous materials, reality by the approach of part supermolecule
The imagination of existing nano-reactor is provided may.8-hydroxyquinoline, many metal complexs of o-phenanthroline all have fluorescence,
8-hydroxyquinoline or o-phenanthroline introduce big ring, and independent due to both having matches somebody with somebody bit function, can form stable oversubscription
Sub- compound, and it is further development of photochemistry device.Four (4- boronates phenyl) porphyrins (TBPP) are in aqueous and sugar
In the presence of son by pi-pi accumulation into aggregation, circular dichroism spectra (CD) exciton coupling band (ECB) symbol, to the absolute of glycan molecule
Configuration has selectivity, can detect the absolute configuration etc. of glycan molecule, supermolecule is had a wide range of applications on analytical chemistry.Oversubscription
The conventional synthetic method of son mainly has following several：Hydro-thermal method, solvent-thermal method, microwave method, ultrasonic synthesis and other conjunctions
Into method.Different synthetic methods frequently results in the product of different structure.In addition, hydro-thermal method or solvent structure products collection efficiency
It is often not high, and contain plurality of impurities or byproduct.
The present invention is disclosed in a kind of cobalt nitrouracil super molecular compound, the compound structure containing free guest molecule
Sub- 5- nitrouracils, the nitrouracil has the acceptor and donor of hydrogen bond, can form specific hydrogen bond with some molecules, from
And make the compound that there is potential application in terms of molecular recognition, Subjective and Objective molecule are exchanged and sensed.In addition, the chemical combination
Contain divalence Co in thing2+Ion, divalence Co2+Ion has d7Valence electron structure, free or underfill electronics unoccupied orbital, energy
D-d transition is formed, thus with abundant electro-chemical activity, so that the compound has in terms of electro-catalysis or mimetic enzyme catalysis
There is potential application.
The content of the invention
The technical problems to be solved by the invention are the preparation process there is provided a kind of reaction condition is gentle for prior art
Simply, with low cost, structural stability is good, containing divalent cobalt ion, 4,4 '-second bipyridine and 5- nitrouracil construction units
Super molecular compound and preparation method thereof.
The present invention is that the technical scheme that solution above-mentioned technical problem is taken is：A kind of cobalt nitrouracil supermolecule chemical combination
Thing, the compound has certain space structure, and its chemical formula is CoC18H32N8O18, its construction unit is [Co (bpy)
(H2O)4]·2(C4H2N3O4)·6H2O (bpy=4,4 '-second bipyridine), crystallographic system is anorthic system, and space group is P-1, structure cell
Parameter isα=86.746 °, β=79.405 °, γ=74.842 °, cobalt from
Son is the octahedra geometric configuration of hexa-coordinate；The nitrouracil is 5- nitrouracils.
A kind of preparation method of above-mentioned cobalt nitrouracil super molecular compound, comprises the following steps：
(1) a certain amount of hydration cobalt acetate and 5- nitroorotic acid potassium monohydrates are weighed, is placed in beaker, according to Co
(II) the amount ratio of ion and the material of 5- nitroorotic acid potassium monohydrates is 1:1 ratio is added, and add water 8~15mL, and is added
Heat, stirring dissolve it, obtain reaction mixture solution；
(2) above-mentioned reaction mixture solution is transferred in the stainless steel cauldron containing 25mL polytetrafluoroethyllining linings,
It is placed in after adding the ethanol of appropriate hydration 4,4 '-second bipyridine and 1~2mL, sealing reactor in air dry oven, 90~
100 DEG C of heating responses 36~48 hours, reaction end is cooled to room temperature, filters out precipitation, and filtrate, which is placed 2~4 days, slowly to be volatilized
Fall partial solvent, obtain red flat crystal；
(3) red flat crystal is taken out, natural air drying, produces described super molecular compound；
It is preferred that, the material for participating in reaction is that chemistry is pure, and the hydration cobalt acetate is four hydration cobalt acetates, hydration
4,4 '-second bipyridine is two 4,4 '-second bipyridines of hydration；
It is preferred that, the amount ratio of the material for participating in reaction is：Cobalt ions: 5- nitroorotic acid potassium monohydrates: hydration
4,4 '-second bipyridine=1: 1: 1.
Compared with prior art, the advantage of the invention is that：
By the nitroorotic acid being conjugated with rigid plane, 4,4 '-second bipyridine part and the cobalt with electro-chemical activity
Ion carries out Supramolecular self assembly reaction, and in the reaction 4,4 '-second bipyridine is used as bridge ligand to connect adjacent cobalt ions shape
Into positively charged one-dimensional chain structure；Decarboxylize forms 5- nitrouracils, 5- nitros to 5- nitroorotic acids in the reaction
Uracil loses a proton and is present in as the anion of monovalence in lattice.Water of coordination molecule, object hydrone and object
5- nitrouracils pass through a variety of hydrogen bonds formation supramolecular network structure.These features cause the super molecular compound negative and positive from
There is potential application prospect in terms of son identification, Subjective and Objective molecule (ion) exchange and electrochemical sensing.
Brief description of the drawings
Fig. 1 be the super molecular compound of the present invention construction unit figure (be illustrative clarity, hydrogen atom, carbon atom and symmetrically
The atom of operation out is not marked)；
Fig. 2 forms two-dimensional network structure figure for the super molecular compound of the present invention in ac.
Embodiment
The present invention is described in further detail below in conjunction with accompanying drawing embodiment.
Embodiment 1：
Weigh Co (Ac)2·4H2O (0.25mmol, 0.0623g), 5- nitro whey potassium monohydrate (0.25mmol,
0.0643g) it is placed in beaker, add water 8mL, heating, stirring dissolve it, obtain reaction mixture solution；Above-mentioned reaction is mixed
Thing solution is transferred in the stainless steel cauldron containing 25mL polytetrafluoroethyllining linings, plus two and is hydrated 4,4 '-second bipyridine
It is placed in after (0.25mmol, 0.0481g), plus ethanol 1mL, sealing reactor in air dry oven, 90 DEG C of heating responses 48 hours,
Reaction end is cooled to room temperature, filters out precipitation, and filtrate is placed and slowly vapors away partial solvent in 4 days, obtains red flat crystal；Will
Red flat crystal takes out, natural air drying, produces described super molecular compound.
Embodiment 2：
Weigh Co (Ac)2·4H2O (0.5mmol, 0.1245g), 5- nitro whey potassium monohydrate (0.5mmol,
0.1286g) it is placed in beaker, add water 10mL, heating, stirring dissolve it, obtain reaction mixture solution；Above-mentioned reaction is mixed
Thing solution is transferred in the stainless steel cauldron containing 25mL polytetrafluoroethyllining linings, plus two and is hydrated 4,4 '-second bipyridine
It is placed in after (0.5mmol, 0.0961g), plus ethanol 2mL, sealing reactor in air dry oven, 95 DEG C of heating responses 40 hours,
Reaction end is cooled to room temperature, filters out precipitation, and filtrate is placed and slowly vapors away partial solvent in 3 days, obtains red flat crystal；Will
Red flat crystal takes out, natural air drying, produces described super molecular compound.
Embodiment 3：
Weigh Co (Ac)2·4H2O (0.5mmol, 0.1245g), 5- nitro whey potassium monohydrate (0.5mmol,
0.1286g) it is placed in beaker, add water 15mL, heating, stirring dissolve it, obtain reaction mixture solution；Above-mentioned reaction is mixed
Thing solution is transferred in the stainless steel cauldron containing 25mL polytetrafluoroethyllining linings, plus two and is hydrated 4,4 '-second bipyridine
It is placed in after (0.5mmol, 0.0961g), plus ethanol 2mL, sealing reactor in air dry oven, 100 DEG C of heating responses 36 hours,
Reaction end is cooled to room temperature, filters out precipitation, and filtrate is placed and slowly vapors away partial solvent in 2 days, obtains red flat crystal；Will
Red flat crystal takes out, natural air drying, produces described super molecular compound.
Super molecular compound made from embodiment 1-3 is subjected to structured testing, as a result shown as described cobalt nitro urine
Pyrimidine super molecular compound, (for illustrative clarity, hydrogen atom, carbon atom and symmetry operation come out its construction unit as shown in Figure 1
Atom do not mark), described cobalt nitrouracil super molecular compound forms two-dimensional network structure such as Fig. 2 institutes in ac
Show.Its chemical formula of super molecular compound obtained by the present invention is CoC18H32N8O18, its construction unit is [Co (bpy)
(H2O)4]·2(C4H2N3O4)·6H2O (bpy=4,4 '-second bipyridine), crystallographic system is anorthic system, and space group is P-1, structure cell
Parameter is α=86.746 °, β=79.405 °, γ=74.842 °, cobalt ions
For the octahedra geometric configuration of hexa-coordinate；In the super molecular compound, 4,4 '-second bipyridine connects phase as bridge ligand
Adjacent cobalt ions forms positively charged one-dimensional chain structure；Decarboxylize forms 5- nitros urine to 5- nitroorotic acids in the reaction
Pyrimidine, 5- nitrouracils lose a proton and are present in as the anion of monovalence in lattice.Water of coordination molecule, object moisture
Son and object 5- nitrouracils pass through a variety of hydrogen bonds formation supramolecular network structure.
Claims (2)
1. a kind of cobalt nitrouracil super molecular compound, it is characterised in that the super molecular compound has certain space structure, it is tied
Structure unit is [Co (bpy) (H2O)4]·2(C4H2N3O4)·6H2O, wherein bpy=4,4 '-second bipyridine, chemical formula is
CoC18H32N8O18, crystallographic system is anorthic system, and space group is P-1, and cell parameter is
α=86.746 °, β=79.405 °, γ=74.842 °, cobalt ions is the octahedra geometric configuration of hexa-coordinate；The nitro urine is phonetic
Pyridine is 5- nitrouracils.
2. a kind of preparation method of cobalt nitrouracil super molecular compound as claimed in claim 1, it is characterised in that including
Following steps：
(1) weigh a certain amount of hydration cobalt acetate and 5- nitroorotic acid potassium monohydrates, be placed in beaker, according to Co (II) from
The amount ratio of son and the material of 5- nitroorotic acid potassium monohydrates is 1:1 ratio is added, and add water 8~15mL, and heat, stir
It is dissolved, reaction mixture solution is obtained；
(2) above-mentioned reaction mixture solution is transferred in the stainless steel cauldron containing 25mL polytetrafluoroethyllining linings, added
It is placed in after appropriate hydration 4,4 '-second bipyridine and 1~2mL ethanol, sealing reactor in air dry oven, 90~100 DEG C
Heating response 36~48 hours, reaction end is cooled to room temperature, filters out precipitation, and filtrate is placed and slowly vapors away part in 2~4 days
Solvent, obtains red flat crystal；
(3) red flat crystal is taken out, natural air drying, produces described super molecular compound；
The material for participating in reaction is that chemistry is pure, and the hydration cobalt acetate is four hydration cobalt acetates, hydration 4,4 '-bigeminy pyrrole
Pyridine is two 4,4 '-second bipyridines of hydration；It is described participate in reaction the amount ratio of material be：Cobalt ions: 5- nitroorotic acid potassium list water
Compound: hydration 4,4 '-second bipyridine=1: 1: 1.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710439529.7A CN107266506B (en) | 2017-06-12 | 2017-06-12 | Cobalt nitrouracil supramolecular compound and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710439529.7A CN107266506B (en) | 2017-06-12 | 2017-06-12 | Cobalt nitrouracil supramolecular compound and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN107266506A true CN107266506A (en) | 2017-10-20 |
| CN107266506B CN107266506B (en) | 2020-05-15 |
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| CN108676020A (en) * | 2018-05-08 | 2018-10-19 | 宁波大学 | A kind of nitrouracil copper super molecular compound and preparation method thereof |
| CN110818746A (en) * | 2019-11-27 | 2020-02-21 | 宁波大学 | 5-nitro orotic acid cobalt complex and preparation method and application thereof |
| CN115403781A (en) * | 2022-10-06 | 2022-11-29 | 北京师范大学 | Room-temperature phosphorescent metal halide crystalline material with reverse excitation wavelength dependence and preparation method thereof |
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| CN103396458A (en) * | 2013-08-12 | 2013-11-20 | 宁波大学 | Compound with electrochemical response to formaldehyde and preparation method thereof |
| CN103435659A (en) * | 2013-08-12 | 2013-12-11 | 宁波大学 | Cobalt complex with electrochemical catalytic activity |
| CN103467367A (en) * | 2013-09-13 | 2013-12-25 | 宁波大学 | Cobalt complex having electrocatalytic activity on hydrogen peroxide |
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| CN103396458A (en) * | 2013-08-12 | 2013-11-20 | 宁波大学 | Compound with electrochemical response to formaldehyde and preparation method thereof |
| CN103435659A (en) * | 2013-08-12 | 2013-12-11 | 宁波大学 | Cobalt complex with electrochemical catalytic activity |
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Cited By (4)
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|---|---|---|---|---|
| CN108676020A (en) * | 2018-05-08 | 2018-10-19 | 宁波大学 | A kind of nitrouracil copper super molecular compound and preparation method thereof |
| CN110818746A (en) * | 2019-11-27 | 2020-02-21 | 宁波大学 | 5-nitro orotic acid cobalt complex and preparation method and application thereof |
| CN115403781A (en) * | 2022-10-06 | 2022-11-29 | 北京师范大学 | Room-temperature phosphorescent metal halide crystalline material with reverse excitation wavelength dependence and preparation method thereof |
| CN115403781B (en) * | 2022-10-06 | 2024-03-19 | 北京师范大学 | Room temperature phosphorescence metal halide crystalline material with reverse excitation wavelength dependence and preparation method thereof |
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