CN104262274A - Lanthanum tetrazolyl-5-formate complex and preparation method thereof - Google Patents

Lanthanum tetrazolyl-5-formate complex and preparation method thereof Download PDF

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Publication number
CN104262274A
CN104262274A CN201410470350.4A CN201410470350A CN104262274A CN 104262274 A CN104262274 A CN 104262274A CN 201410470350 A CN201410470350 A CN 201410470350A CN 104262274 A CN104262274 A CN 104262274A
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China
Prior art keywords
tetrazole
formic acid
lanthanide complex
complex
acid lanthanide
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CN201410470350.4A
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Inventor
张秀清
刘汉甫
范超逸
李璇
张淑华
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Guilin University of Technology
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Guilin University of Technology
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Priority to CN201410470350.4A priority Critical patent/CN104262274A/en
Publication of CN104262274A publication Critical patent/CN104262274A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07FACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F5/00Compounds containing elements of Groups 3 or 13 of the Periodic Table
    • C07F5/003Compounds containing elements of Groups 3 or 13 of the Periodic Table without C-Metal linkages
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D257/00Heterocyclic compounds containing rings having four nitrogen atoms as the only ring hetero atoms
    • C07D257/02Heterocyclic compounds containing rings having four nitrogen atoms as the only ring hetero atoms not condensed with other rings
    • C07D257/04Five-membered rings
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07FACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F5/00Compounds containing elements of Groups 3 or 13 of the Periodic Table

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)

Abstract

The invention discloses a lanthanum tetrazolyl-5-formate complex and a preparation method thereof. The lanthanum complex is prepared from carboxylate anions with higher coordination capacity by a solution process. The method has the advantages of simple technique, low cost, favorable repetitiveness and the like; and the successfully synthesized lanthanum complex provides certain references for synthesis of the rare-earth metal complex.

Description

Tetrazole-5-formic acid Lanthanide complex and preparation method thereof
Technical field
The invention belongs to complex preparation technical field, particularly a kind of tetrazole-5-formic acid Lanthanide complex and preparation method thereof.
Background technology
The title complex of rare earth metal, due to the physical properties of its uniqueness and chemical property, has important strategic position in 21 century.Radius is large owing to having for rare earth ion, ligancy high and cause the interest of many chemists.The formation of rare earth metal complex is subject to the impact of all many condition, the ratio, reaction conditions etc. of the character of such as part, the coordination configuration of metal ion, metal-salt and part.Therefore, when synthesizing rare-earth metal complexes, the selection of part is very important.As everyone knows, carboxylic acid is a good part, plays a part very important in coordination chemistry.Carboxylic acid has diversified coordination mode, comprises monodentate ligand, bidentate bridging, chelating ligands, chelating bridging etc.This paper for part, has synthesized Rare Earth Lanthanum title complex with tetrazole-5-formic acid.
Summary of the invention
The object of this invention is to provide a kind of tetrazole-5-formic acid Lanthanide complex and preparation method thereof.
Thinking of the present invention: the carboxylate anion utilizing coordination ability strong obtains Lanthanide complex by solution method.
The structural formula of tetrazole-5-formic acid Lanthanide complex of the present invention is:
In this tetrazole-5-formic acid Lanthanide complex, part participates in coordinations with four tooth pattern of chelating between two, central metallic ions La (III) is respectively with from four nitrogen-atoms of four parts, four Sauerstoffatoms, and the nitrogen-atoms oxygen atom ligand having a part of vibration, ligancy is ten; Ligating atom forms the anti-prism structure in two cap four directions around La (III) ion, and by the chelating bridge linking effect of part, La (III) ion is connected to space three-dimensional structure.
The preparation method of above-mentioned tetrazole-5-formic acid Lanthanide complex is:
(1) weigh 0.5 ~ 2mmol tetrazole-5-ethyl formate to be dissolved in 5 ~ 10mL distilled water, add 0.5 ~ 2mmol KOH, stirred at ambient temperature 2 ~ 4 hours, obtained mixing solutions.
(2) in the obtained mixing solutions of step (1), 0.1 ~ 0.4mmol LaCl is added 37H 2o, stirred at ambient temperature 2 ~ 3 hours, obtains white casse liquid, filters obtained colourless solution.
(3) colourless solution obtained for step (2) is placed in beaker seals with preservative film, seven or eight apertures pricked by preservative film, be placed in the good cupboard that ventilates to leave standstill and separate out colourless bulk crystals after three months, be tetrazole-5-formic acid Lanthanide complex.
Method of the present invention has simple, the with low cost and reproducible advantage of technique, and the Lanthanide complex that success is synthesized is that the title complex of synthesizing rare-earth metal provides certain foundation.
Accompanying drawing explanation
Fig. 1 is the molecular structure of tetrazole-5-formic acid Lanthanide complex of the present invention.
Embodiment
Embodiment:
(1) weigh 0.1420 gram of tetrazole-5-ethyl formate (1mmol) to be dissolved in 10mL distilled water, add 0.0560 gram of KOH (1mmol), stirred at ambient temperature 3 hours, obtained mixing solutions.
(2) in the obtained mixing solutions of step (1), 0.0743 gram of LaCl is added 37H 2o (0.2mmol), stirred at ambient temperature 2 hours, obtains white casse liquid, filters obtained colourless solution.
(3) colourless solution obtained for step (2) is placed in beaker seals with preservative film, seven apertures pricked by preservative film, be placed in the good cupboard that ventilates to leave standstill and separate out colourless bulk crystals after three months, be tetrazole-5-formic acid Lanthanide complex.Its structure is:
In this tetrazole-5-formic acid Lanthanide complex, part participates in coordinations with four tooth pattern of chelating between two.Central metallic ions La (III) is respectively with from four nitrogen-atoms of four parts, and four Sauerstoffatoms, and the nitrogen-atoms oxygen atom ligand having a part of vibration, ligancy is ten.Ligating atom forms the anti-prism structure in two cap four directions around La (III) ion.By the chelating bridge linking effect of part, La (III) ion is connected to space three-dimensional structure.

Claims (2)

1. a tetrazole-5-formic acid Lanthanide complex, is characterized in that the structural formula of described tetrazole-5-formic acid Lanthanide complex is:
In this tetrazole-5-formic acid Lanthanide complex, part participates in coordinations with four tooth pattern of chelating between two, central metallic ions La (III) is respectively with from four nitrogen-atoms of four parts, four Sauerstoffatoms, and the nitrogen-atoms oxygen atom ligand having a part of vibration, ligancy is ten; Ligating atom forms the anti-prism structure in two cap four directions around La (III) ion, and by the chelating bridge linking effect of part, La (III) ion is connected to space three-dimensional structure.
2. the preparation method of tetrazole-5-formic acid Lanthanide complex according to claim 1, is characterized in that concrete steps are:
(1) weigh 0.5 ~ 2mmol tetrazole-5-ethyl formate to be dissolved in 5 ~ 10mL distilled water, add 0.5 ~ 2mmol KOH, stirred at ambient temperature 2 ~ 4 hours, obtained mixing solutions;
(2) in the obtained mixing solutions of step (1), 0.1 ~ 0.4mmol LaCl is added 37H 2o, stirred at ambient temperature 2 ~ 3 hours, obtains white casse liquid, filters obtained colourless solution;
(3) colourless solution obtained for step (2) is placed in beaker seals with preservative film, seven or eight apertures pricked by preservative film, be placed in the good cupboard that ventilates to leave standstill and separate out colourless bulk crystals after three months, be tetrazole-5-formic acid Lanthanide complex.
CN201410470350.4A 2014-09-15 2014-09-15 Lanthanum tetrazolyl-5-formate complex and preparation method thereof Pending CN104262274A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108384020A (en) * 2018-03-09 2018-08-10 河海大学 It is a kind of novel containing the metal organic framework for not being coordinated tetrazole group and its synthetic method and application
CN110041352A (en) * 2019-05-21 2019-07-23 中北大学 Tetrazoleacetic acid lanthanum energetic compound synthetic method and its influence that HMX is thermally decomposed

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101993689A (en) * 2009-08-25 2011-03-30 中国科学院福建物质结构研究所 Rare-earth metal coordination polymer fluorescence luminescent material, and synthesis and application thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101993689A (en) * 2009-08-25 2011-03-30 中国科学院福建物质结构研究所 Rare-earth metal coordination polymer fluorescence luminescent material, and synthesis and application thereof

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
张秀清: "四氮唑羧酸配合物的合成及其性质研究", 《中国博士学位论文全文数据库 工程科技I辑》 *
李超: "含四氟对苯二甲胺Schiff碱及其配合物的合成、结构及性质的研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 *
沈菲: "苯胺-2,5-二磺酸配合物的合成和性质研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 *
陈蔷薇等: "氨基酸-镧配合物的合成及单晶培养研究", 《广州化工》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108384020A (en) * 2018-03-09 2018-08-10 河海大学 It is a kind of novel containing the metal organic framework for not being coordinated tetrazole group and its synthetic method and application
CN108384020B (en) * 2018-03-09 2020-09-11 河海大学 Metal organic framework containing uncoordinated tetrazole group and synthesis method and application thereof
CN110041352A (en) * 2019-05-21 2019-07-23 中北大学 Tetrazoleacetic acid lanthanum energetic compound synthetic method and its influence that HMX is thermally decomposed

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Application publication date: 20150107