CN108404991A - A kind of catalysis oxidation purposes of sulfaquinoxaline cobalt compound - Google Patents
A kind of catalysis oxidation purposes of sulfaquinoxaline cobalt compound Download PDFInfo
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- CN108404991A CN108404991A CN201810432762.7A CN201810432762A CN108404991A CN 108404991 A CN108404991 A CN 108404991A CN 201810432762 A CN201810432762 A CN 201810432762A CN 108404991 A CN108404991 A CN 108404991A
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- cobalt
- sulfaquinoxaline
- compound
- cobalt compound
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- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 21
- 230000003647 oxidation Effects 0.000 title claims abstract description 20
- 229960003097 sulfaquinoxaline Drugs 0.000 title claims abstract description 19
- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 15
- -1 sulfaquinoxaline cobalt compound Chemical class 0.000 title claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- NHZLNPMOSADWGC-UHFFFAOYSA-N 4-amino-N-(2-quinoxalinyl)benzenesulfonamide Chemical compound C1=CC(N)=CC=C1S(=O)(=O)NC1=CN=C(C=CC=C2)C2=N1 NHZLNPMOSADWGC-UHFFFAOYSA-N 0.000 claims abstract description 11
- 150000001869 cobalt compounds Chemical class 0.000 claims abstract description 9
- 150000001875 compounds Chemical class 0.000 claims abstract description 7
- 150000001868 cobalt Chemical class 0.000 claims abstract description 5
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000013078 crystal Substances 0.000 claims description 14
- 239000003054 catalyst Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 229910017052 cobalt Inorganic materials 0.000 claims description 7
- 239000010941 cobalt Substances 0.000 claims description 7
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 7
- 235000019441 ethanol Nutrition 0.000 claims description 7
- 239000012046 mixed solvent Substances 0.000 claims description 7
- 239000003446 ligand Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 3
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid group Chemical group C(C1=CC=CC=C1)(=O)O WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 2
- 229940011182 cobalt acetate Drugs 0.000 claims description 2
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 2
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 2
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims 3
- 241000208340 Araliaceae Species 0.000 claims 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 claims 1
- 235000003140 Panax quinquefolius Nutrition 0.000 claims 1
- 125000002252 acyl group Chemical group 0.000 claims 1
- 235000008434 ginseng Nutrition 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 17
- 235000015511 Liquidambar orientalis Nutrition 0.000 abstract description 5
- 230000010718 Oxidation Activity Effects 0.000 abstract description 5
- 241000736148 Styrax Species 0.000 abstract description 5
- 239000004870 Styrax Substances 0.000 abstract description 5
- 235000000126 Styrax benzoin Nutrition 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 239000011149 active material Substances 0.000 abstract 1
- 239000007800 oxidant agent Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 239000002262 Schiff base Substances 0.000 description 6
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical compound N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 description 5
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 4
- 229910001429 cobalt ion Inorganic materials 0.000 description 4
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000001590 oxidative effect Effects 0.000 description 4
- 150000004753 Schiff bases Chemical class 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- VEUMANXWQDHAJV-UHFFFAOYSA-N 2-[2-[(2-hydroxyphenyl)methylideneamino]ethyliminomethyl]phenol Chemical compound OC1=CC=CC=C1C=NCCN=CC1=CC=CC=C1O VEUMANXWQDHAJV-UHFFFAOYSA-N 0.000 description 2
- 206010015856 Extrasystoles Diseases 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000021615 conjugation Effects 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 2
- SMQUZDBALVYZAC-UHFFFAOYSA-N salicylaldehyde Chemical compound OC1=CC=CC=C1C=O SMQUZDBALVYZAC-UHFFFAOYSA-N 0.000 description 2
- FDDDEECHVMSUSB-UHFFFAOYSA-N sulfanilamide Chemical compound NC1=CC=C(S(N)(=O)=O)C=C1 FDDDEECHVMSUSB-UHFFFAOYSA-N 0.000 description 2
- 229940124530 sulfonamide Drugs 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- WNSYXLVRJPORMB-UHFFFAOYSA-N N1=CC=CC2=CC=CC=C12.[Co] Chemical compound N1=CC=CC2=CC=CC=C12.[Co] WNSYXLVRJPORMB-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- WURBFLDFSFBTLW-UHFFFAOYSA-N benzil Chemical compound C=1C=CC=CC=1C(=O)C(=O)C1=CC=CC=C1 WURBFLDFSFBTLW-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000006735 epoxidation reaction Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- MMIPFLVOWGHZQD-UHFFFAOYSA-N manganese(3+) Chemical compound [Mn+3] MMIPFLVOWGHZQD-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/18—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms
- B01J31/1805—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms the ligands containing nitrogen
- B01J31/181—Cyclic ligands, including e.g. non-condensed polycyclic ligands, comprising at least one complexing nitrogen atom as ring member, e.g. pyridine
- B01J31/1825—Ligands comprising condensed ring systems, e.g. acridine, carbazole
- B01J31/183—Ligands comprising condensed ring systems, e.g. acridine, carbazole with more than one complexing nitrogen atom, e.g. phenanthroline
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/27—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation
- C07C45/32—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen
- C07C45/37—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of >C—O—functional groups to >C=O groups
- C07C45/39—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of >C—O—functional groups to >C=O groups being a secondary hydroxyl group
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2231/00—Catalytic reactions performed with catalysts classified in B01J31/00
- B01J2231/70—Oxidation reactions, e.g. epoxidation, (di)hydroxylation, dehydrogenation and analogues
- B01J2231/76—Dehydrogenation
- B01J2231/763—Dehydrogenation of -CH-XH (X= O, NH/N, S) to -C=X or -CX triple bond species
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/02—Compositional aspects of complexes used, e.g. polynuclearity
- B01J2531/0238—Complexes comprising multidentate ligands, i.e. more than 2 ionic or coordinative bonds from the central metal to the ligand, the latter having at least two donor atoms, e.g. N, O, S, P
- B01J2531/0241—Rigid ligands, e.g. extended sp2-carbon frameworks or geminal di- or trisubstitution
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/80—Complexes comprising metals of Group VIII as the central metal
- B01J2531/84—Metals of the iron group
- B01J2531/845—Cobalt
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of catalysis oxidation purposes of sulfaquinoxaline cobalt compound, feature is that the compound is a kind of cobalt compound to styrax with catalytic oxidation activity, molecular formula C38H32N10O5S2Co, crystallographic system are monocline, and space group is P2 (1)/c, cell parameterα=90 °, β=100.848 °, γ=90 °.The compound is by cobalt salt, sulfaquinoxaline and 2, and 2 ' second bipyridines are mixed in a certain ratio reaction and are made, and has specific space structure and accurate molecular formula, synthesis step simple.Cobalt compound produced by the present invention shows good catalytic oxidation activity to styrax, has broad application prospects as potential catalytically-active materials.
Description
Technical field
The invention belongs to technical field of material chemistry more particularly to a kind of catalysis oxidation purposes of sulfaquinoxaline cobalt compound.
Background technology
Catalytic oxidation is one of most important reaction in chemical industry, field of medicaments.In early stage catalytic oxidation
The oxidant of use is mostly all kinds of inorganic compound oxidants, such as potassium permanganate, potassium bichromate, these oxidants are to environment dirt
Dye is serious.As environmental problem has been to be concerned by more and more people, environmentally friendly Green Oxidant (such as oxygen, peroxidating
Hydrogen, ozone etc.) receive the favor of people, it has also become the research hotspot of oxidation reaction.However, this kind of oxidant there are oxidisability not
By force, the deficiencies of oxidation susceptibility is uncertain, reaction condition is complicated.The study found that under the action of some complex catalyst,
The Green Oxidants such as oxygen have good catalysed oxidn.Therefore, the ligand compound that selective catalysis is efficient, selectivity is good
Object catalyst is one of the effective way for realizing catalytic oxidation.
Transition metal complex compound can be used as effective catalyst, be the electro catalytic activity because of central ion, due to mistake
Crossing has vacant d tracks and not pairs of d electronics in the atomic structure of metal, pass through catalyst and reactant containing transition metal
The contact of molecule, will form the chemical bonds of various features on the vacant d tracks of these catalyst to achieve the purpose that molecule activation, from
And reduce the activation energy of complex reaction, change the approach of reaction, and the ligand with conjugation group then can active centre from
Son is conducive to the transmission of electronics, makes it have good catalytic activity.Schiff base metal complex (Salen complexs) has
Reversible bioactivity shows good catalytic oxidation performance (Yuan Zeli etc., asymmetric schiff bases in some catalytic oxidations
The synthesis of Cu (H) complex and catalytic performance research [J], using chemical industry, 2009,38 (4), 547~550).Zhao uses after congruent people
Alanine-schiff base of salicylaldehyde manganese (III) complex as catalyst realize to epoxidation reaction of olefines (catalysis journal,
2005,26 (7), 571~576).Jin Chun et al. has studied the structure and catalytic of asymmetric cobalt Salen type schiff bases complexes
Energy (Acta PhySico-Chimica Sinica, 2006,2,22 (8), 947~952).Above-mentioned schiff base metal complex is as existing for catalyst
Problem is the deficiencies of part schiff bases synthetic yield is not high, stability is bad or of high cost.Some primitives of conjugation containing rigidity have
Machine ligand can form the complex of stable structure with transition metal ions, and have good catalytic oxidation performance.This
Invention prepares a kind of cobalt coordination compound using sulfaquinoxaline as ligand, with divalent cobalt ion central ion, which prepares
Method is simple, structure and performance are stablized, and has potential application prospect as catalytic oxidant.
Invention content
The technical problem to be solved by the present invention is to be directed to the prior art, provide it is a kind of to styrax with catalysis oxidation live
The sulfaquinoxaline cobalt compound of property, the catalytic oxidation have the characteristics that step is simple, reaction condition temperature.
Technical solution is used by the present invention solves above-mentioned technical problem：A kind of catalysis of sulfaquinoxaline cobalt compound
Purposes is aoxidized, which is a kind of cobalt complex compound to styrax with good catalysis oxidation, abbreviation sulfanilamide (SN) Kui Evil
Quinoline cobalt compound, skeleton symbol are [Co (L)2(bpy)]·H2O (L=sloughs the sulfaquinoxaline of a proton, bpy=2,
2 '-second bipyridines), molecular formula C38H32N10O5S2Co, crystallographic system are monocline, and space group is P2 (1)/c, cell parameterα=90 °, β=100.848 °, γ=90 °, cobalt ions are deformation eight
The geometric configuration of face body coordination, two of which nitrogen coordination atom come from 2,2 '-second bipyridines, and four nitrogen coordination atoms come from
Two sulfaquinoxalines.The preparation method is former by nitrogen in cobalt ions and sulfaquinoxaline and 2,2 '-second bipyridine ligands
Coordination between son forms the cobalt compound of mononuclear structure, specifically includes following steps：
By cobalt salt, sulfaquinoxaline and 2,2 '-second bipyridines in molar ratio 1:2:1 ratio mixing be dissolved in water, ethyl alcohol and
The in the mixed solvent of DMF, forms mixture solution, and water, ethyl alcohol and DMF volume ratios are 2:4:1；
Said mixture solution microwave heating is stirred, 15~30min of back flow reaction postcoolings to room temperature, is stood, slowly
Red bulk crystals are precipitated in solvent flashing 2~4 days；
Above-mentioned red bulk crystals are tested with X-ray single crystal diffractometer, obtain the brilliant bag parameter of red bulk crystals
Forα=90 °, β=100.848 °, γ=90 °, crystallographic system are monocline,
Space group is P2 (1)/c, and above-mentioned red bulk crystals are a kind of complex of cobalt, abbreviation cobalt compound.
Optionally, the sulfaquinoxaline, abbreviation HL, molecular formula C14H12N4O2S, structural formula are：
Optionally, the cobalt salt for participating in reaction is one or more of cobaltous sulfate, cobalt nitrate or cobalt acetate；
The DMF is the abbreviation of N,N-dimethylformamide；
The substance for participating in reaction is that chemistry is pure.
Compared with the prior art, the advantages of the present invention are as follows：By sulfaquinoxaline and 2,2 '-bigeminy with a conjugated structure
Pyridine is coordinated with the cobalt ions with catalytic oxidation activity, and a kind of cobalt coordination compound is made, which has accurately empty
Between structure (Fig. 1) and accurate molecular formula；Prepared cobalt compound stability of material is high, has good catalysis to styrax
Oxidation activity has potential application prospect as catalytic oxidation activity material.
Description of the drawings
Fig. 1 is the structural unit figure of the cobalt compound of the present invention, and for the sake of clarity hydrogen atom is omitted, and O5 is object water
Molecule.
Specific implementation mode
Present invention is further described in detail with reference to embodiments.
Embodiment 1：
Weigh CoSO4·6H2O (0.263g, 1.0mmol), sulfaquinoxaline (0.600g, 2.0mmol), 2,2 '-bigeminy
The in the mixed solvent of pyridine (0.156g, 1.0mmol) plus 4.0mL distilled water, 8mL ethyl alcohol and 2.0mL DMF, then microwave heating
Stirring, back flow reaction 15min postcoolings to room temperature are stood, and red bulk crystals are precipitated after 2 days in slow solvent flashing.
Embodiment 2：
Weigh [Co (NO3)2]·6H2O (0.291g, 1.0mmol), sulfaquinoxaline (0.600g, 2.0mmol), 2,2 '-
The in the mixed solvent of second bipyridine (0.156g, 1.0mmol) plus 6.0mL distilled water, 12mL ethyl alcohol and 3.0mL DMF, it is then micro-
Wave heating stirs, back flow reaction 30min postcoolings to room temperature, stands, and slow solvent flashing is precipitated red blocky brilliant after 3 days
Body.
Embodiment 3：
Weigh Co (Ac)2·4H2O (0.249g, 1.0mmol), sulfaquinoxaline (0.600g, 2.0mmol), 2,2 '-two
Bipyridyl (0.156g, 1.0mmol) adds the in the mixed solvent of 8.0mL distilled water, 16mL ethyl alcohol and 4.0mL DMF, then microwave
Heating stirring, back flow reaction 20min postcoolings to room temperature are stood, and red bulk crystals are precipitated after 4 days in slow solvent flashing.
Red bulk crystals progress X-ray single crystal diffractometer analysis test obtained, determines its molecule in above-described embodiment
Formula is C38H32N10O5S2Co, crystallographic system are monocline, and space group is P2 (1)/c, cell parameter α=90 °, β=100.848 °, γ=90 °, the i.e. complex of cobalt, structural unit such as Fig. 1 institutes
Show.
Using the cobalt compound obtained by above-described embodiment as the benzoic catalyst of catalysis oxidation, in ethyl alcohol and water volume
Than being 1:2 in the mixed solvent, 45 DEG C of reaction 40min under air atmosphere, the yield of benzil product up to 76.5% or more,
Catalytic oxidation formula is as follows, which has potential application as catalysis oxidation agent material.
。
Claims (2)
1. a kind of catalysis oxidation purposes of sulfaquinoxaline cobalt compound, which is characterized in that the cobalt compound is as catalysis oxidation
Benzoic catalyst is 1 in ethyl alcohol and water volume ratio:2 in the mixed solvent, 45 DEG C of reaction 40min, benzene under air atmosphere
The yield of even acyl product is up to 76.5% or more.
2. the catalysis oxidation purposes of sulfaquinoxaline cobalt compound according to claim 1, which is characterized in that the cobalt
The preparation method for closing object includes the following steps：
1) by cobalt salt, sulfaquinoxaline and 2,2 '-second bipyridines in molar ratio 1:2:1 ratio mixing is dissolved in water, ethyl alcohol and DMF
In the mixed solvent, formed mixture solution, water, ethyl alcohol and DMF volume ratios be 2:4:1；
2) said mixture solution microwave heating is stirred, 15~30min of back flow reaction postcoolings to room temperature, stands, slowly waves
It sends out solvent 2~4 days, red bulk crystals is precipitated；
3) test analysis is carried out to above-mentioned red bulk crystals with X-ray single crystal diffractometer, obtains the brilliant packet ginseng of red bulk crystals
Number isα=90 °, β=100.848 °, γ=90 °, crystallographic system are single
Tiltedly, space group is P2 (1)/c, molecular formula C38H32N10O5S2Co, the red bulk crystals are a kind of ligand compound of cobalt
Object, abbreviation cobalt compound；
The cobalt salt for participating in reaction is one or more of cobaltous sulfate, cobalt nitrate or cobalt acetate；
The DMF is the abbreviation of N,N-dimethylformamide；
The substance for participating in reaction is that chemistry is pure.
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| DD144759A1 (en) * | 1979-07-10 | 1980-11-05 | Peter Palitzsch | METHOD FOR PRODUCING BENZIL |
| CN102476063A (en) * | 2010-11-30 | 2012-05-30 | 中国科学院大连化学物理研究所 | Bifunctional catalyst and application of bifunctional catalyst in preparation of benzil by benzoin dehydrogenation/oxidation |
| CN103159607A (en) * | 2011-12-12 | 2013-06-19 | 中国科学院大连化学物理研究所 | Method for preparing benzil by oxidizing benzoin with molecular oxygen |
| CN103467367A (en) * | 2013-09-13 | 2013-12-25 | 宁波大学 | Cobalt complex having electrocatalytic activity on hydrogen peroxide |
| CN107903155A (en) * | 2017-11-23 | 2018-04-13 | 大连理工大学 | A kind of method that catalysis oxidation styrax prepares benzil |
-
2018
- 2018-05-08 CN CN201810432762.7A patent/CN108404991B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
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