CN117986164A - A method for preparing copper ethyl sulfate tetrahydrate complex crystal - Google Patents
A method for preparing copper ethyl sulfate tetrahydrate complex crystal Download PDFInfo
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- CN117986164A CN117986164A CN202410081386.7A CN202410081386A CN117986164A CN 117986164 A CN117986164 A CN 117986164A CN 202410081386 A CN202410081386 A CN 202410081386A CN 117986164 A CN117986164 A CN 117986164A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C305/00—Esters of sulfuric acids
- C07C305/02—Esters of sulfuric acids having oxygen atoms of sulfate groups bound to acyclic carbon atoms of a carbon skeleton
- C07C305/04—Esters of sulfuric acids having oxygen atoms of sulfate groups bound to acyclic carbon atoms of a carbon skeleton being acyclic and saturated
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- 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
- C07F1/00—Compounds containing elements of Groups 1 or 11 of the Periodic Table
- C07F1/005—Compounds containing elements of Groups 1 or 11 of the Periodic Table without C-Metal linkages
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- 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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Abstract
一种四水合硫酸乙酯铜配合物晶体化合物合成方法是称取双(苯乙酰)二硫化物(0.3020g，1mmol)置于100ml圆底烧瓶中，加入20ml无水乙醇搅拌使其溶解，再将Cu(NO3)2·3H2O(0.4834g，2mmol)乙醇(30ml)溶液加入到上述溶液中，100℃下回流反应24小时，反应结束后趁热过滤，在空气中自然挥发，3天后，有蓝色晶体析出，其分子结构式如下：
A synthesis method of a tetrahydrate ethyl sulfate copper complex crystalline compound is as follows: weigh bis(phenylacetyl) disulfide (0.3020 g, 1 mmol) and place it in a 100 ml round-bottom flask, add 20 ml of anhydrous ethanol and stir to dissolve it, then add Cu(NO 3 ) 2 ·3H 2 O (0.4834 g, 2 mmol) ethanol (30 ml) solution to the above solution, reflux at 100° C. for 24 hours, filter while hot after the reaction is completed, evaporate naturally in the air, and after 3 days, blue crystals are precipitated, and the molecular structure thereof is as follows:
Description
Technical Field
The invention relates to a metal organic coordination compound (complex) and a preparation method thereof, in particular to a nitrogen-containing oxazoline metal organic complex and a preparation method thereof, and specifically relates to an oxazoline copper complex and a synthesis method thereof.
Background
With the development of organic chemistry, the metal organic compound is increasingly widely applied to organic synthesis, is one of the fields which are very active in the organic chemistry at present, and has been widely applied to organic synthesis reactions. Asymmetric synthesis reactions catalyzed by chiral ligands and transition metal complexes, which occur later in the 60 s of the 20 th century, greatly accelerate the study of chiral drugs.
Reference is made to:
1.Zhang,Xiao;Xue,Jinchun;Han,Huaqin;Wang,Yu,Study on improvement of copper sulfide acid soil properties and mechanism of metal ion fixation based on Fe-biochar composite,Scientific Reports(2024),14(1),247.
2.Vimala,T.M.;Swaminathan,S.Crystal structure of copper ethyl sulfate tetrahydrate,Current Science(1969),38(15),362.
Disclosure of Invention
The invention aims to provide a Cu-N metal organic complex for being applied to the field of catalysis, and aims to solve the technical problem of selecting aniline as a ligand to synthesize a copper complex of bisoxazoline in one step.
The invention relates to a tetrahydrated ethyl sulfate copper complex, which is a complex prepared from bis (phenylacetyl) disulfide and copper nitrate trihydrate in an ethanol solvent and shown by the following chemical formula:
Chemical name: copper ethyl sulfate tetrahydrate complex, complex (I) for short.
The synthesis method comprises the steps of synthesis and separation, wherein bis (phenylacetyl) disulfide (0.3020 g,1 mmol) is weighed and placed in a 100ml round bottom flask, 20ml absolute ethyl alcohol is added and stirred to dissolve the bis (phenylacetyl) disulfide, then Cu (NO 3)2·3H2 O (0.4834 g,2 mmol) ethanol (30 ml) solution is added into the solution, reflux reaction is carried out for 24 hours at 100 ℃, filtering is carried out when the reaction is finished, natural volatilization is carried out in air, and blue crystals are separated out after 3 days.
The synthesis reaction is as follows:
The synthesis method obtains the target product in one step, and has simple process and convenient operation.
The reaction mechanism of the reaction is that the bis (phenylacetyl) disulfide is broken by S-S bond under the action of Lewis acid copper nitrate trihydrate, and stable tetrahydrate copper ethyl sulfate complex is formed in one step. The mechanism of formation and energy variation of this mechanism are under investigation.
Drawings
FIG. 1 is an X-ray diffraction analysis chart of a copper ethyl sulfate tetrahydrate complex.
Detailed Description
Weighing bis (phenylacetyl) disulfide (0.3020 g,1 mmol) and placing in a 100ml round bottom flask, adding 20ml anhydrous ethanol, stirring to dissolve, adding Cu (NO 3)2·3H2 O (0.4834 g,2 mmol) ethanol (30 ml) solution into the above solution, reflux reacting at 100deg.C for 24 hr, filtering while hot, naturally volatilizing in air, precipitating blue crystal after 3 days, melting point of 88-90deg.C, yield of 52%
Elemental analysis data C 4 H18CuO12S2, found: 12.83% of C; h:4.650% of the total weight of the product; s:15.605% of the total weight of the product; theoretical value: 12.44 percent of C; h is 4.665%; s:16.621% of the total weight of the product; infrared spectroscopic data (KBr, cm -1): 3491;2990;2889;3256;1661;1056;999;762;592.
The complex crystal data are as follows:
typical bond length data for crystals:
Typical bond angle data for crystals:
Claims (1)
1. A method for synthesizing a compound having the following structural formula and unit cell parameters: comprises synthesis, separation and purification, wherein bis (phenylacetyl) disulfide (0.3020 g,1 mmol) is weighed and placed in a 100ml round bottom flask, 20ml absolute ethyl alcohol is added and stirred to dissolve the bis (phenylacetyl) disulfide, cu (NO 3)2·3H2 O (0.4834 g,2 mmol) ethanol (30 ml) is added into the solution, reflux reaction is carried out for 24 hours at 100 ℃, filtration is carried out when the reaction is finished, natural volatilization is carried out in air, blue crystals are separated out after 3 days, the compound crystal (I) is obtained by using MoK alpha rays which are monochromatized by a graphite monochromator on an oxford X-ray single crystal diffractometer at 296 (2) K temperature Collecting diffraction data in an omega-theta scanning mode, wherein the method is characterized by comprising the following steps of: the crystal belongs to monoclinic system, P21/C, unit cell parameters: /(I)α＝90°；β＝93.645(2)°；Gamma=90°, its molecular structural formula is as follows:
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| CN202410081386.7A CN117986164A (en) | 2024-01-19 | 2024-01-19 | A method for preparing copper ethyl sulfate tetrahydrate complex crystal |
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| CN202410081386.7A CN117986164A (en) | 2024-01-19 | 2024-01-19 | A method for preparing copper ethyl sulfate tetrahydrate complex crystal |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103709047A (en) * | 2014-01-14 | 2014-04-09 | 罗梅 | Chiral (R)-phenylethylamine hydrochloride copper chloride complex |
| WO2015085522A1 (en) * | 2013-12-11 | 2015-06-18 | Evonik Industries Ag | Process for preparing alkanesulphonic acids |
| CN107759497A (en) * | 2017-10-18 | 2018-03-06 | 辽宁省轻工设计院有限公司 | A kind of method of synthesizing methyl sulfonic acid |
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- 2024-01-19 CN CN202410081386.7A patent/CN117986164A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015085522A1 (en) * | 2013-12-11 | 2015-06-18 | Evonik Industries Ag | Process for preparing alkanesulphonic acids |
| CN103709047A (en) * | 2014-01-14 | 2014-04-09 | 罗梅 | Chiral (R)-phenylethylamine hydrochloride copper chloride complex |
| CN107759497A (en) * | 2017-10-18 | 2018-03-06 | 辽宁省轻工设计院有限公司 | A kind of method of synthesizing methyl sulfonic acid |
Non-Patent Citations (4)
| Title |
|---|
| C. S. BRUSCHIN1 ET AL.: "THE STRUCTURE OF COPPER(II) DODECYLSULPHATE TETRAHYDRATE", POLYHEDRON, vol. 14, 31 December 1995 (1995-12-31), pages 3099 - 3016 * |
| MARIYA KHITERER ET AL.: "Hybrid Polyelectrolyte Materials for Fuel Cell Applications: Design, Synthesis, and Evaluation of Proton-Conducting Bridged Polysilsesquioxanes", CHEM. MATER., vol. 18, 31 December 2006 (2006-12-31), pages 3665 - 3673, XP055535825, DOI: 10.1021/cm060440a * |
| N. WATANABE ET AL.: "Chemical Environment of Copper Aggregates Embedded in Polypyrrole Films: The Nature of the Copper-Polypyrrole Interaction", J. PHYS. CHEM. B, vol. 106, 31 December 2002 (2002-12-31), pages 11102 - 11107 * |
| VINALA.T.M ET AL.: "Crystal structure of copper ethyl sulfate tetrahydrate.", CURRENT SCIENCE, vol. 38, no. 15, 31 December 1969 (1969-12-31), pages 362 * |
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Inventor after: Luo Mei Inventor after: Yang Yanting Inventor after: Hu Baiquan Inventor after: Zhang Jingcheng Inventor before: Luo Mei Inventor before: Yang Yanting Inventor before: Hu Baiquan Inventor before: Zhang Jingcheng |
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