CN108440581B - 一种5-硝基乳清酸单核锌配合物及其制备方法和用途 - Google Patents
一种5-硝基乳清酸单核锌配合物及其制备方法和用途 Download PDFInfo
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- WJFDCFHWFHCLIW-UHFFFAOYSA-N 2-(bromomethyl)-6-methylpyridine Chemical compound CC1=CC=CC(CBr)=N1 WJFDCFHWFHCLIW-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 239000011701 zinc Substances 0.000 title claims abstract description 28
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 238000010668 complexation reaction Methods 0.000 title description 2
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 claims abstract description 27
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- 239000013078 crystal Substances 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims abstract description 9
- 230000003197 catalytic effect Effects 0.000 claims abstract description 5
- 150000003751 zinc Chemical class 0.000 claims abstract description 5
- 229910052751 metal Inorganic materials 0.000 claims abstract description 4
- 239000002184 metal Substances 0.000 claims abstract description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 23
- 239000000203 mixture Substances 0.000 claims description 12
- OPGJGRWULGFTOS-UHFFFAOYSA-N 5-nitro-2,4-dioxo-1h-pyrimidine-6-carboxylic acid Chemical compound OC(=O)C=1NC(=O)NC(=O)C=1[N+]([O-])=O OPGJGRWULGFTOS-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- ISAOCJYIOMOJEB-UHFFFAOYSA-N benzoin Chemical compound C=1C=CC=CC=1C(O)C(=O)C1=CC=CC=C1 ISAOCJYIOMOJEB-UHFFFAOYSA-N 0.000 claims description 8
- YNPNZTXNASCQKK-UHFFFAOYSA-N Phenanthrene Natural products C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 claims description 7
- 239000000725 suspension Substances 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 125000004430 oxygen atom Chemical group O* 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- -1 zinc 5-nitroorotate Chemical compound 0.000 claims description 5
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 5
- 244000028419 Styrax benzoin Species 0.000 claims description 4
- 235000000126 Styrax benzoin Nutrition 0.000 claims description 4
- 235000008411 Sumatra benzointree Nutrition 0.000 claims description 4
- 125000004429 atom Chemical group 0.000 claims description 4
- WURBFLDFSFBTLW-UHFFFAOYSA-N benzil Chemical compound C=1C=CC=CC=1C(=O)C(=O)C1=CC=CC=C1 WURBFLDFSFBTLW-UHFFFAOYSA-N 0.000 claims description 4
- 229960002130 benzoin Drugs 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 235000019382 gum benzoic Nutrition 0.000 claims description 4
- 239000003446 ligand Substances 0.000 claims description 4
- 239000012046 mixed solvent Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 4
- 125000004433 nitrogen atom Chemical group N* 0.000 claims description 3
- 239000011592 zinc chloride Substances 0.000 claims description 3
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
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- 239000004246 zinc acetate Substances 0.000 claims description 2
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- PXQPEWDEAKTCGB-UHFFFAOYSA-N orotic acid Chemical compound OC(=O)C1=CC(=O)NC(=O)N1 PXQPEWDEAKTCGB-UHFFFAOYSA-N 0.000 description 23
- 229960005010 orotic acid Drugs 0.000 description 12
- 239000001257 hydrogen Substances 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 239000003814 drug Substances 0.000 description 4
- 229940079593 drug Drugs 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 150000001661 cadmium Chemical class 0.000 description 2
- 210000004027 cell Anatomy 0.000 description 2
- 239000002537 cosmetic Substances 0.000 description 2
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- 229910021645 metal ion Inorganic materials 0.000 description 2
- HWCXJKLFOSBVLH-UHFFFAOYSA-N 5-amino-2,4-dioxo-1h-pyrimidine-6-carboxylic acid Chemical compound NC1=C(C(O)=O)NC(=O)NC1=O HWCXJKLFOSBVLH-UHFFFAOYSA-N 0.000 description 1
- WCQOZELYYCFURJ-UHFFFAOYSA-L C(C1=CC(=O)NC(=O)N1)(=O)[O-].[Ni+2].C(C1=CC(=O)NC(=O)N1)(=O)[O-] Chemical compound C(C1=CC(=O)NC(=O)N1)(=O)[O-].[Ni+2].C(C1=CC(=O)NC(=O)N1)(=O)[O-] WCQOZELYYCFURJ-UHFFFAOYSA-L 0.000 description 1
- 206010008909 Chronic Hepatitis Diseases 0.000 description 1
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- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 230000019522 cellular metabolic process Effects 0.000 description 1
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- 208000019423 liver disease Diseases 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
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- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000013343 vitamin Nutrition 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
- C07F3/00—Compounds containing elements of Groups 2 or 12 of the Periodic Table
- C07F3/06—Zinc compounds
-
- 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
- B01J31/22—Organic complexes
- B01J31/2204—Organic complexes the ligands containing oxygen or sulfur as complexing atoms
- B01J31/2208—Oxygen, e.g. acetylacetonates
- B01J31/2217—At least one oxygen and one nitrogen atom present as complexing atoms in an at least bidentate or bridging ligand
-
- 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
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- 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
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- 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
- B01J2531/0213—Complexes without C-metal linkages
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- 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
- B01J2531/20—Complexes comprising metals of Group II (IIA or IIB) as the central metal
- B01J2531/26—Zinc
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Nitrogen Condensed Heterocyclic Rings (AREA)
Abstract
本发明公开了一种5‑硝基乳清酸单核锌配合物及其制备方法和用途，该配合物是由锌盐、5‑硝基乳清酸以及1,10‑邻菲罗啉为原料通过自组装反应制备而得，具有明确的空间结构和准确的分子式，合成步骤简单。其结构单元由一个金属锌离子、一个5‑硝基乳清酸根、一个1,10‑邻菲罗啉、一个配位水分子组成，其分子式为C17H11N5O7Zn，晶系为三斜，空间群为P‑1，
α＝71.106°，β＝77.759°，γ＝75.990°。所制备的配合物是一种催化氧化剂材料，具有优异的物化性能，在催化材料领域具有广阔的应用前景。
Description
技术领域
本发明属于配位化学领域，具体涉及一种5-硝基乳清酸单核锌配合物及其制备方法和用途。
背景技术
近年来，乳清酸及其衍生物已经成为国内外生物医药界研究的热点。乳清酸及其衍生物在医药领域的用途相当广泛，例如其对脂肪肝、黄疸性肝病和急慢性肝炎均有较好的疗效。在日本乳清酸主要用于复合维生素的非处方药物的成分和清凉饮料的添加剂；在西欧，它不仅是医药维生素的组成，而且广泛应用于化妆品中，作为营养型化妆品基质，可以被皮肤细胞吸收，促进细胞的新陈代谢，抑制皮肤衰老；在美国人们对乳清酸及其衍生物的研究较多。国内外已经开发出以乳清酸为基础的系列化药物，如硝基乳清酸、氨基乳清酸等。乳清酸及其衍生物具有非对称的空间结构和多种配位官能团，能够和不同的金属离子形成丰富多样的配位化合物。目前，国内外文献报道了一些乳清酸类药物与金属的配合物，这不仅大大丰富了乳清酸类药物配位化学的发展，同时也为挖掘乳清酸及其衍生物在其它方面的应用提供了可能。乳清酸及其衍生物的金属配合物在光电材料领域也显示出潜在的应用前景。中国专利(胡秀峰等，CN102329610B)公开了一种紫色荧光材料，该材料是基于5-硝基乳清酸的镉配合物；殷艺晅等人公开了一种乳清酸镍配合物(一种双核镍配合物及其制备方法，申请号为2017104399847)；在中国化学会第27届学术年会第08分会场摘要集(2010)公开了5-硝基乳清酸Cd(II)化合物，在第十六届全国金属有机化学学术讨论会论文集(2010)公开了5-氨基乳清酸二核、四核镉簇合物。李星等人报道了一系列5-硝基乳清酸的镉配合物(CrystEngComm.,2011,13(21),6373–6376)，其中部分配合物具有较强的荧光发射性能。5-硝基乳清酸具有不同的配位原子，多个配位点以及非对称的几何结构，为结构类型的多样性提供了可能，分子中同时存在氢键给体和受体，有利于形成超分子网络。本发明通过5-硝基乳清酸、1,10-邻菲罗啉与过渡金属锌离子通过自组装反应制备了一种5-硝基乳清酸单核锌配合物，该配合物具有的明确空间结构和准确的分子式，分子中具有多个氢键给体和受体，通过氢键或π-π堆积作用能够形成三维超分子网络，该配合物具有良好的物理化学性能，在药物研究、光电材料或催化材料领域具有广阔的应用前景。
发明内容
本发明是针对现有技术中存在的问题，提供5-硝基乳清酸单核锌配合物及其制备方法。
本发明为解决上述技术问题所采用的技术方案为：一种5-硝基乳清酸单核锌配合物，该配合物的结构单元是由一个金属锌离子、一个5-硝基乳清酸根(HL2-)、一个1,10-邻菲罗啉(phen)、一个配位水分子组成，其结构简式为[Zn(HL)(phen)(H2O)]，分子式为C17H11N5O7Zn，所属晶系为三斜，空间群为P-1，晶胞参数
α＝71.106°，β＝77.759°，γ＝75.990°；锌离子为五配位的几何构型，其中两个氮配位原子来自于1,10-邻菲罗啉配体，一个氧原子和一个氮原子来自5-硝基乳清酸根，一个氧原子来自配位水分子，结构单元如图1所示。
本发明还提供了所述的5-硝基乳清酸单核锌配合物的制备方法，所述制备方法包括以下步骤：
取锌盐、5-硝基乳清酸和1,10-邻菲罗啉(phen)置于圆底烧瓶中，加体积比为10～20:1的蒸馏水和DMF，其中，Zn(II)离子、5-硝基乳清酸、1,10-邻菲罗啉的摩尔比为1:1:1，室温搅拌10min形成混合物悬浊液，转移到不锈钢反应釜中70～100oC反应24～48h，自然冷却至室温，过滤分离，得无色块状晶体，即为所述5-硝基乳清酸单核锌配合物；
所述5-硝基乳清酸简写为H3L，分子式为C5H3N3O6，其结构式为
所述HL2-为失去两个H+的5-硝基乳清酸根；所述DMF为N,N-二甲基甲酰胺的简称；所述phen为1,10-邻菲罗啉的简称；
所述锌盐为氯化锌、醋酸锌或硝酸锌中的一种或几种；
所述参加反应的物质或溶剂均为化学纯。
进一步的，本发明还提供了所述的5-硝基乳清酸单核锌配合物的用途，该锌配合物作为催化氧化安息香的催化剂，在乙醇和水体积比为1:4的混合溶剂中50oC、反应30min后，苯偶酰的收率达到65％以上。
与现有技术相比，本发明的优点在于：
将具有共轭结构的1,10-邻菲罗啉和具有嘧啶环结构的5-硝基乳清酸与锌离子配位，制得5-硝基乳清酸单核锌配合物，该配合物具有准确的空间结构(图1)和准确的分子式；1,10-邻菲罗啉具有大的共轭平面，能产生π-π作用，以及5-硝基乳清酸提供氢键给体和受体，可形成分子间氢键，借助特有的分子间力、π-π和氢键的作用该配合物能够形成特定三维超分子网络；锌离子和配体都具有光电活性，使得该化合物具有优异的物化性能，其作为催化氧化安息香的催化剂，在乙醇和水混合溶剂中50oC、反应30min后，苯偶酰的收率达到65％以上，因此，该配合物在光电材料和催化材料领域具有广阔的应用前景。
附图说明
图1为本发明的5-硝基乳清酸单核锌配合物的结构单元。
具体实施方式
以下结合实施例对本发明作进一步详细描述。
实施例1：
称取ZnCl2(0.136g，1.0mmol)、5-硝基乳清酸(0.201g，1.0mmol)、1,10-邻菲罗啉(0.180g，1.0mmol)置于圆底烧瓶中，加蒸馏水10mL和DMF 1.0mL，室温搅拌10min形成混合物悬浊液，然后转移到不锈钢反应釜中70oC反应48h，自然冷却至室温，过滤分离，得无色块状晶体。
实施例2：
称取Zn(OAc)2·2H2O(0.438g，2.0mmol)、5-硝基乳清酸(0.402g，2.0mmol)、1,10-邻菲罗啉(0.360g，2.0mmol)置于圆底烧瓶中，加蒸馏水20mL和DMF 1.0mL，室温搅拌10min形成混合物悬浊液，然后转移到不锈钢反应釜中100oC反应24h，自然冷却至室温，过滤分离，得无色块状晶体。
实施例3：
称取Zn(NO3)2·6H2O(0.297g，1.0mmol)、5-硝基乳清酸(0.201g，1.0mmol)、1,10-邻菲罗啉(0.180g，1.0mmol)置于圆底烧瓶中，加蒸馏水15mL和DMF 1mL，室温搅拌10min形成混合物悬浊液，然后转移到不锈钢反应釜中90oC反应36h，自然冷却至室温，过滤分离，得无色块状晶体。
将上述实施例中制得的无色块状晶体进行X射线单晶衍射测试分析，经测定其结构单元是由一个金属锌离子、一个5-硝基乳清酸根、一个1,10-邻菲罗啉、一个配位水分子组成，结构简式为[Zn(HL)(phen)(H2O)]，分子式为C17H11N5O7Zn，晶系为三斜，空间群为P-1，晶胞参数
α＝71.106°，β＝77.759°，γ＝75.990°；锌离子为五配位的几何构型，其中两个氮配位原子来自于1,10-邻菲罗啉配体，一个氧原子和一个氮原子来自5-硝基乳清酸根，一个氧原子来自配位水分子，结构单元如图1所示，所制得无色块状晶体即为所述5-硝基乳清酸单核锌配合物。
将所制得的5-硝基乳清酸单核锌配合物作为催化氧化安息香的催化剂，在乙醇和水体积比为1:4的混合溶剂中50oC、反应30min后，苯偶酰的收率达到65％以上。
Claims (3)
1.一种5-硝基乳清酸单核锌配合物，其特征在于，该配合物的结构单元是由一个金属锌离子、一个5-硝基乳清酸根、一个1,10-邻菲罗啉、一个配位水分子组成，其结构简式为[Zn(HL)(phen)(H2O)]，分子式为C17H11N5O7Zn，晶系为三斜，空间群为P-1，
α＝71.106°，β＝77.759°，γ＝75.990°；锌离子为五配位的几何构型，其中两个氮配位原子来自于1,10-邻菲罗啉配体，一个氧原子和一个氮原子来自5-硝基乳清酸根，一个氧原子来自配位水分子；
所述HL为失去两个H+的5-硝基乳清酸根；
所述phen为1,10-邻菲罗啉的简称。
2.一种权利要求1所述的5-硝基乳清酸单核锌配合物的制备方法，其特征在于，所述制备方法包括以下步骤：
取锌盐、5-硝基乳清酸和1,10-邻菲罗啉置于圆底烧瓶中，加体积比为10～20:1的蒸馏水和DMF，其中，Zn(II)离子、5-硝基乳清酸、1,10-邻菲罗啉的摩尔比为1:1:1，室温搅拌10min形成混合物悬浊液，转移到不锈钢反应釜中70～100℃反应24～48h，自然冷却至室温，过滤分离，得无色块状晶体，即为所述5-硝基乳清酸单核锌配合物；
所述锌盐为氯化锌、醋酸锌或硝酸锌中的一种或几种；
所述DMF为N,N-二甲基甲酰胺的简称；
所述参加反应的物质或溶剂均为化学纯。
3.根据权利要求1所述的5-硝基乳清酸单核锌配合物的用途，其特征在于，该锌配合物作为催化氧化安息香的催化剂，在乙醇和水体积比为1:4的混合溶剂中50℃、反应30min后，苯偶酰的收率达到65％以上。
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