CN108586503A - 4’-苯基-2,2′:6′,2′′-三联吡啶硝酸钕配合物的制备方法 - Google Patents
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 229910017604 nitric acid Inorganic materials 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims abstract description 13
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 10
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 9
- USJZIUVMYSUNGB-UHFFFAOYSA-N neodymium;hydrate Chemical compound O.[Nd] USJZIUVMYSUNGB-UHFFFAOYSA-N 0.000 claims abstract description 7
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 claims abstract description 4
- 239000013078 crystal Substances 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 3
- -1 nitrate ions Chemical class 0.000 claims description 9
- 229910002651 NO3 Inorganic materials 0.000 claims description 8
- 239000003446 ligand Substances 0.000 claims description 4
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims description 4
- 125000004433 nitrogen atom Chemical group N* 0.000 claims description 4
- 239000013522 chelant Substances 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 2
- 125000004429 atom Chemical group 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 238000005303 weighing Methods 0.000 claims 1
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 5
- 150000002910 rare earth metals Chemical class 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 4
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 238000013329 compounding Methods 0.000 description 2
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 210000003739 neck Anatomy 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 239000000700 radioactive tracer Substances 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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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
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
- C07F5/003—Compounds containing elements of Groups 3 or 13 of the Periodic Table without C-Metal linkages
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pyridine Compounds (AREA)
Abstract
本发明公开了一种4'‑苯基‑2,2′:6′,2′′‑三联吡啶硝酸钕配合物的制备方法。称量4'‑苯基‑2,2′:6′,2′′‑三联吡啶溶解于二氯甲烷中制得溶液,将溶液移入反应釜内;称量六水合硝酸钕溶解于乙腈中制得六水合硝酸钕溶液,将六水合硝酸钕溶液加入反应釜中,然后将反应釜置于电热鼓风干燥箱中,在80℃下恒温反应48小时,最后冷却至室温,得到粉红色针状晶体,即为4'‑苯基‑2,2′:6′,2′′‑三联吡啶硝酸钕配合物;该配合物属于正交晶系,空间群为Pbca。本发明具有工艺简单、成本低廉、重复性好等优点,成功的合成了钕配合物,为合成稀土金属的配合物提供了一定的依据。
Description
技术领域
本发明属于配合物制备技术领域,特别涉及一种4'-苯基-2,2′:6′,2′′-三联吡啶硝酸钕配合物的制备方法。
背景技术
稀土配合物因其独特的光致发光性质,在生物探针、分析传感、光电转换等诸多领域有着潜在的应用价值。并且稀土配合物单色性好、荧光寿命长、Stoke位移大,与含N、S的生物大分子如蛋白质、DNA有很好的亲和性,可作为生物探针,被广泛地应用于结构探针、分子开关、示踪试剂、抑菌活动等方面。稀土金属Nd、4'-苯基-2,2′:6′,2′′-三联吡啶形成的配合物存在丰富多样的结构,对于设计合成目标结构的配合物很有研究意义。
发明内容
本发明的目的是提供一种4'-苯基-2,2′:6′,2′′-三联吡啶硝酸钕配合物的制备方法。
本发明的思路:以4'-苯基-2,2′:6′,2′′-三联吡啶为配体与六水合硝酸钕通过溶剂热法获得钕配合物。
具体步骤为:
(1) 称量0.1~0.12毫摩尔4'-苯基-2,2′:6′,2′′-三联吡啶溶解于3~6毫升二氯甲烷中制得溶液,将溶液移入容积为25毫升的反应釜内。
(2) 称量0.1~0.12毫摩尔六水合硝酸钕溶解于1~2毫升乙腈中制得六水合硝酸钕溶液,将六水合硝酸钕溶液加入步骤(1)的反应釜中,然后将反应釜置于电热鼓风干燥箱中,在80℃下恒温反应48小时,最后冷却至室温,得到粉红色针状晶体,即为4'-苯基-2,2′:6′,2′′-三联吡啶硝酸钕配合物,该4'-苯基-2,2′:6′,2′′-三联吡啶硝酸钕配合物的结构为:
。
该4'-苯基-2,2′:6′,2′′-三联吡啶硝酸钕配合物属于正交晶系,空间群为Pbca,基本结构单元中包含一个钕离子,一个4'-苯基-2,2′:6′,2′′-三联吡啶分子,三个硝酸根离子和一个水分子;中心Nd(Ⅲ)离子分别与4'-苯基-2,2′:6′,2′′-三联吡啶中性配体的三个氮原子以三齿螯合的形式配位,与三个硝酸根离子以双齿螯合的形式配位,与水分子配位,形成了十配位的双帽十二面体构型;Nd-O键长是2.482~2.611 Ǻ,Nd-N键长是2.522~2.2559 Ǻ。
所述三个氮原子为N1、N2、N3;所述三个硝酸根离子为O1和O3、O4和O6、O7和O9;所述水分子为O10。
本发明具有工艺简单、成本低廉、重复性好等优点,成功的合成了钕配合物,为合成稀土金属的配合物提供了一定的依据。
附图说明
图1是本发明中4'-苯基-2,2′:6′,2′′-三联吡啶硝酸钕配合物的分子结构图。
图2是本发明中4'-苯基-2,2′:6′,2′′-三联吡啶硝酸钕配合物的三维堆积图。
具体实施方式
实施例:
(1) 称量0.1毫摩尔(0.0313克)4'-苯基-2,2′:6′,2′′-三联吡啶溶解于6毫升二氯甲烷中制得溶液,将溶液移入容积为25毫升的反应釜内。
(2) 称量0.1毫摩尔(0.0437克)六水合硝酸钕溶解于2毫升乙腈中制得六水合硝酸钕溶液,将六水合硝酸钕溶液加入步骤(1)的反应釜中,然后将反应釜置于电热鼓风干燥箱中,在80℃下恒温反应48小时,最后冷却至室温,得到粉红色针状晶体,即为4'-苯基-2,2′:6′,2′′-三联吡啶硝酸钕配合物,该4'-苯基-2,2′:6′,2′′-三联吡啶硝酸钕配合物的结构为:
。
该4'-苯基-2,2′:6′,2′′-三联吡啶硝酸钕配合物属于正交晶系,空间群为Pbca,基本结构单元中包含一个钕离子,一个4'-苯基-2,2′:6′,2′′-三联吡啶分子,三个硝酸根离子和一个水分子。中心Nd(Ⅲ)离子分别与4'-苯基-2,2′:6′,2′′-三联吡啶中性配体的三个氮原子(N1、N2、N3)以三齿螯合的形式配位,与三个硝酸根离子(O1、O3;O4、O6;O7、O9)以双齿螯合的形式配位,与水分子(O10)配位,形成了十配位的双帽十二面体构型。Nd-O键长是2.482~2.611 Ǻ,Nd-N键长是2.522~2.2559 Ǻ。
Claims (1)
1.一种4'-苯基-2,2′:6′,2′′-三联吡啶硝酸钕配合物的制备方法,其特征在于具体步骤为:
(1) 称量0.1~0.12毫摩尔4'-苯基-2,2′:6′,2′′-三联吡啶溶解于3~6毫升二氯甲烷中制得溶液,将溶液移入容积为25毫升的反应釜内;
(2) 称量0.1~0.12毫摩尔六水合硝酸钕溶解于1~2毫升乙腈中制得六水合硝酸钕溶液,将六水合硝酸钕溶液加入步骤(1)的反应釜中,然后将反应釜置于电热鼓风干燥箱中,在80℃下恒温反应48小时,最后冷却至室温,得到粉红色针状晶体,即为4'-苯基-2,2′:6′,2′′-三联吡啶硝酸钕配合物,该4'-苯基-2,2′:6′,2′′-三联吡啶硝酸钕配合物的结构为:
;
该4'-苯基-2,2′:6′,2′′-三联吡啶硝酸钕配合物属于正交晶系,空间群为Pbca,基本结构单元中包含一个钕离子,一个4'-苯基-2,2′:6′,2′′-三联吡啶分子,三个硝酸根离子和一个水分子;中心Nd(Ⅲ)离子分别与4'-苯基-2,2′:6′,2′′-三联吡啶中性配体的三个氮原子以三齿螯合的形式配位,与三个硝酸根离子以双齿螯合的形式配位,与水分子配位,形成了十配位的双帽十二面体构型;Nd-O键长是2.482~2.611 Ǻ,Nd-N键长是2.522~2.2559Ǻ;
所述三个氮原子为N1、N2、N3;所述三个硝酸根离子为O1和O3、O4和O6、O7和O9;所述水分子为O10。
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EP3862349A1 (en) * | 2020-02-10 | 2021-08-11 | Merck Patent GmbH | Hydrated crystalline polynuclear metal complex, hydrated crystalline polynuclear metal complex including a guest compound analyte and its use in a method for determining molecular structure of the guest compound analyte |
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EP3862349A1 (en) * | 2020-02-10 | 2021-08-11 | Merck Patent GmbH | Hydrated crystalline polynuclear metal complex, hydrated crystalline polynuclear metal complex including a guest compound analyte and its use in a method for determining molecular structure of the guest compound analyte |
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