CN103087108B - 2-[nitrogen-(triphenylmethyl) imino-] pyridine-2-chromium nitrate salt compound and preparation method thereof - Google Patents
2-[nitrogen-(triphenylmethyl) imino-] pyridine-2-chromium nitrate salt compound and preparation method thereof Download PDFInfo
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- CN103087108B CN103087108B CN201210491202.1A CN201210491202A CN103087108B CN 103087108 B CN103087108 B CN 103087108B CN 201210491202 A CN201210491202 A CN 201210491202A CN 103087108 B CN103087108 B CN 103087108B
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- triphenylmethyl
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Abstract
It is simple that the present invention discloses a kind of working method, 2-[nitrogen-(triphenylmethyl) imino-] pyridine-2-chromium nitrate salt compound that preparation time is short and cheap, its preparation method is dissolved respectively in organic solvent [nitrogen-(triphenylmethyl) imino-] pyridine and chromium nitrate, stir at 15 ~ 25 DEG C of temperature, obtain the saturated solution of two kinds of compounds respectively, be 1: 1 mixing by volume by these two kinds of saturated solutions, stir 30 minutes, cover with normal hexane, 2 weeks are left standstill under 15 ~ 25 DEG C of temperature condition, obtain 2-[nitrogen-(triphenylmethyl) imino-] pyridine-2-chromium nitrate salt compound crystal, described organic solvent is ethanol or tetrahydrofuran (THF), molecular structure skeleton symbol is as follows.
Description
Technical field
The present invention relates to mineral compound that a kind of macromolecular ligand coordination obtains and preparation method thereof, especially a kind of working method is simple, 2-[nitrogen-(triphenylmethyl) imino-] pyridine-2-chromium nitrate salt compound that preparation time is short and cheap and preparation method thereof.
Background technology
Due to the mineral compound obtained with macromolecular ligand coordinations such as [nitrogen-(triphenylmethyl) imino-] pyridines, there are excellent microporosity, molecular magnetism and linear optics etc., have broad application prospects, therefore, people more and more pay attention to the research to ligand polymer quasi-molecule.Such as brave (the Yong Fang in side in 2006, Cui-Ying Huang, Zai-Ming Zhu, Xiao-Li Yu and Wan-Sheng You, Acta Crystallographica Section E, 2006, E62, m3347-3348) etc. people's report take [nitrogen-(triphenylmethyl) imino-] pyridine as the cobalt compounds etc. of part synthesis.But because macromolecular ligand (comprising [nitrogen-(triphenylmethyl) imino-] pyridine) its steric effect is comparatively large, be difficult to synthesize ligand polymer quickly and efficiently, this is also be the difficult problem perplexing people always.
Summary of the invention
The present invention is the above-mentioned technical problem in order to solve existing for prior art, provides a kind of working method simple, 2-[nitrogen-(triphenylmethyl) imino-] pyridine-2-chromium nitrate salt compound that preparation time is short and cheap and preparation method thereof.
Technical solution of the present invention is: a kind of 2-[nitrogen-(triphenylmethyl) imino-] pyridine-2-chromium nitrate salt compound, it is characterized in that the molecular structure skeleton symbol of described 2-[nitrogen-(triphenylmethyl) imino-] pyridine-2-chromium nitrate salt compound is as follows:
。
Described 2-[nitrogen-(triphenylmethyl) imino-] pyridine-2-chromium nitrate salt compound, it is characterized in that: the outward appearance of described 2-[nitrogen-(triphenylmethyl) imino-] pyridine-2-chromium nitrate salt compound is diamond platy crystal, crystalline structure is oblique system, spacer is P2 (1)/n, lattice parameter a=10.287, b=23.462, c=17.868, α=γ=90 °, β=105.266 °.
The preparation method of a kind of above-mentioned 2-[nitrogen-(triphenylmethyl) imino-] pyridine-2-chromium nitrate salt compound, it is characterized in that carrying out as follows: [nitrogen-(triphenylmethyl) imino-] pyridine and chromium nitrate are dissolved in organic solvent respectively, stir at 15 ~ 25 DEG C of temperature, obtain the saturated solution of two kinds of compounds respectively, be 1:1 mixing by volume by these two kinds of saturated solutions, stir 30 minutes, cover with normal hexane, 2 weeks are left standstill under 15 ~ 25 DEG C of temperature condition, obtain 2-[nitrogen-(triphenylmethyl) imino-] pyridine-2-chromium nitrate salt compound crystal, described organic solvent is ethanol or tetrahydrofuran (THF).
The present invention is simple to operate, preparation time is short (2 weeks), efficiency is high, only common whipping appts is needed in preparation process, prepared product, except having excellent microporosity the same as existing macromolecular ligand coordination mineral compound, molecular magnetism and linear optics, also has the advantages such as cheap.
Accompanying drawing explanation
Fig. 1 is the molecular structure that the product of the embodiment of the present invention is analyzed through X-ray diffraction.
Fig. 2 is that the products molecule of the embodiment of the present invention is along a direction of principal axis accumulation graph.
Embodiment
Embodiment 1:
[nitrogen-(triphenylmethyl) imino-] pyridine and chromium nitrate dissolve in ethanol by preparation method respectively, stir at 20 ~ 25 DEG C of temperature, obtain the saturated solution of two kinds of compounds respectively, be 1:1 mixing by volume by these two kinds of saturated solutions, stir 30 minutes, cover with normal hexane, under 20 ~ 25 DEG C of temperature condition, leave standstill 2 weeks, obtain 2-[nitrogen-(triphenylmethyl) imino-] pyridine-2-chromium nitrate salt compound crystal.
Embodiment 2:
[nitrogen-(triphenylmethyl) imino-] pyridine and chromium nitrate are dissolved in tetrahydrofuran (THF) by preparation method respectively, stir at 15 ~ 20 DEG C of temperature, obtain the saturated solution of two kinds of compounds respectively, be 1:1 mixing by volume by these two kinds of saturated solutions, stir 30 minutes, cover with normal hexane, under 15 ~ 20 DEG C of temperature condition, leave standstill 2 weeks, obtain 2-[nitrogen-(triphenylmethyl) imino-] pyridine-2-chromium nitrate salt compound crystal.
As shown in Figure 1, molecular structure sketch is as follows for the molecular structure that 2-[nitrogen-(triphenylmethyl) imino-] pyridine-2-chromium nitrate salt compound crystal embodiment 1 or embodiment 2 obtained is analyzed through X-ray diffraction:
2-[nitrogen-(triphenylmethyl) imino-] pyridine-2-chromium nitrate salt compound crystal outward appearance that embodiment 1 or embodiment 2 obtain is diamond platy crystal, crystalline structure is oblique system, spacer is P2 (1)/n, lattice parameter a=10.287, b=23.462, c=17.868, α=γ=90 °, β=105.266 °.Crystal molecule along a direction of principal axis accumulation graph as shown in Figure 2.
Claims (2)
1. 2-[nitrogen-(triphenylmethyl) imino-] pyridine-2-chromium nitrate salt compound, is characterized in that the molecular structure skeleton symbol of described 2-[nitrogen-(triphenylmethyl) imino-] pyridine-2-chromium nitrate salt compound is as follows:
；
The outward appearance of described 2-[nitrogen-(triphenylmethyl) imino-] pyridine-2-chromium nitrate salt compound is diamond platy crystal, crystalline structure is oblique system, spacer is P2 (1)/n, lattice parameter a=10.287, b=23.462, c=17.868, α=γ=90 °, β=105.266 °.
2. the preparation method of 2-as claimed in claim 1 [nitrogen-(triphenylmethyl) imino-] pyridine-2-chromium nitrate salt compound, it is characterized in that carrying out as follows: [nitrogen-(triphenylmethyl) imino-] pyridine and chromium nitrate are dissolved in organic solvent respectively, stir at 15 ~ 25 DEG C of temperature, obtain the saturated solution of two kinds of compounds respectively, be 1:1 mixing by volume by these two kinds of saturated solutions, stir 30 minutes, cover with normal hexane, 2 weeks are left standstill under 15 ~ 25 DEG C of temperature condition, obtain 2-[nitrogen-(triphenylmethyl) imino-] pyridine-2-chromium nitrate salt compound crystal, described organic solvent is ethanol or tetrahydrofuran (THF).
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1568285A (en) * | 2001-10-12 | 2005-01-19 | 韩国Nano技术株式会社 | Synthesis of mono-disperse and highly crystalline nano-particles of metals, alloys, metal-oxides, and multi-metallic oxides without a size-selection process |
| WO2009033183A2 (en) * | 2007-09-08 | 2009-03-12 | University Of Florida Research Foundation | Compounds and methods for treatment of hcv and conditions associated with cd81 binding |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1568285A (en) * | 2001-10-12 | 2005-01-19 | 韩国Nano技术株式会社 | Synthesis of mono-disperse and highly crystalline nano-particles of metals, alloys, metal-oxides, and multi-metallic oxides without a size-selection process |
| WO2009033183A2 (en) * | 2007-09-08 | 2009-03-12 | University Of Florida Research Foundation | Compounds and methods for treatment of hcv and conditions associated with cd81 binding |
Non-Patent Citations (3)
| Title |
|---|
| Dichloridobis{2-[(triphenylmethyl)-amino]pyridine-κN}cadmium(II);Guang-Ning Zhang;《Acta Crystallographic a Section E》;20081231;第m357页 * |
| Yong Fang等,.Dichlorobis{2-[(triphenylmethyl )amino]pyridyl}-cobalt(II).《Acta Crystallographic a Section E》.2006,第m3347-m3348页. * |
| 孙亚光等,.配合物[Cr3(μ3-O)(Tc)6(H2O)3].(NO3).4H2O的水热合成及晶体结构.《无机化学学报》.2008,第24卷(第12期),第2039-2042页. * |
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