CN106967123A - 一种甲苯与4,4’‑联吡啶构筑的锰配合物及合成方法 - Google Patents
一种甲苯与4,4’‑联吡啶构筑的锰配合物及合成方法 Download PDFInfo
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- CN106967123A CN106967123A CN201710242063.1A CN201710242063A CN106967123A CN 106967123 A CN106967123 A CN 106967123A CN 201710242063 A CN201710242063 A CN 201710242063A CN 106967123 A CN106967123 A CN 106967123A
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- bpy
- mnl
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- bipyridyl
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- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000010189 synthetic method Methods 0.000 title claims abstract description 9
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 6
- 229910052748 manganese Inorganic materials 0.000 title claims abstract description 6
- 239000011572 manganese Substances 0.000 title claims abstract description 6
- MWVTWFVJZLCBMC-UHFFFAOYSA-N 4,4'-bipyridine Chemical compound C1=NC=CC(C=2C=CN=CC=2)=C1 MWVTWFVJZLCBMC-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000013078 crystal Substances 0.000 claims abstract description 17
- 239000000178 monomer Substances 0.000 claims abstract description 6
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 claims abstract description 5
- PQLVXDKIJBQVDF-UHFFFAOYSA-N acetic acid;hydrate Chemical class O.CC(O)=O PQLVXDKIJBQVDF-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 5
- 239000011737 fluorine Substances 0.000 claims abstract description 5
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims abstract description 5
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims abstract description 4
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000004821 distillation Methods 0.000 claims 1
- 239000003643 water by type Substances 0.000 abstract description 3
- 239000000470 constituent Substances 0.000 abstract description 2
- 238000000034 method Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- -1 (4 carboxybenzyl) amino Chemical group 0.000 abstract 2
- 238000004458 analytical method Methods 0.000 abstract 1
- 238000010586 diagram Methods 0.000 description 3
- 238000000547 structure data Methods 0.000 description 3
- 239000013256 coordination polymer Substances 0.000 description 2
- 229920001795 coordination polymer Polymers 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- RDRCCJPEJDWSRJ-UHFFFAOYSA-N pyridine;1h-pyrrole Chemical compound C=1C=CNC=1.C1=CC=NC=C1 RDRCCJPEJDWSRJ-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
Classifications
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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
- C07F13/00—Compounds containing elements of Groups 7 or 17 of the Periodic Table
- C07F13/005—Compounds without a metal-carbon linkage
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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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pyridine Compounds (AREA)
Abstract
4‑(N,N’‑双(4‑羧基苄基)氨基)甲苯与4,4’‑联吡啶构筑的锰配合物[MnL(4,4’‑bpy)0.5]n及合成方法。其特征在于[MnL(4,4’‑bpy)0.5]n的单体分子式为：C28H23MnN2O4，分子量为：506.42g/mol,H2L为分析纯4‑(N,N’‑双(4‑羧基苄基)氨基)甲苯，4,4’‑bpy为分析纯4,4’‑联吡啶。将0.094‑0.188g分析纯H2L和0.039‑0.078g分析纯4,4’‑联吡啶溶于10‑20mL二次蒸馏水中，调节pH为7后，再加入0.061‑0.122g分析纯四水合乙酸锰，置于聚氟四乙烯高压反应釜中，并置于180℃烘箱三天后取出，冷却至室温，打开高压反应釜，底部有浅粉色透明块状晶体即[MnL(4,4’‑bpy)0.5]n。本发明工艺简单、成本低廉、化学组分易于控制、重复性好且产量高。
Description
技术领域
4-(N,N’-双(4-羧基苄基)氨基)甲苯与4,4’-联吡啶构筑的锰配合物[MnL(4,4’-bpy)0.5]n(H2L为分析纯4-(N,N’-双(4-羧基苄基)氨基)甲苯，4,4’-bpy为分析纯4,4’-联吡啶)及合成方法。
背景技术
配位聚合物(coordination polymer)是进十几年配位化学发展的最快的一个方向，是一个涉及无机化学、有机化学和配位化学等多学科的崭新的研究课题。兼有无机材料的刚性和有机材料的柔性特征，使其在现代材料研究方面呈现出巨大的发展潜力和诱人的发展前景。
发明内容
本发明的目的就是为设计合成新型的4-(N,N’-双(4-羧基苄基)氨基)甲苯与4,4’-联吡啶构筑的锰配合物，利用溶剂热法合成[MnL(4,4’-bpy)0.5]n。
本发明涉及的[MnL(4,4’-bpy)0.5]n的单体分子式为：C28H23MnN2O4，分子量为：506.42g/mol,H2L为分析纯4-(N,N’-双(4-羧基苄基)氨基)甲苯，4,4’-bpy为分析纯4,4’-联吡啶。晶体结构数据见表一,键长键角数据见表二。
表一[MnL(4,4’-bpy)0.5]n的晶体学参数
表二[MnL(4,4’-bpy)0.5]n的部分键长和键角(°)
所述[MnL(4,4’-bpy)0.5]n的合成方法具体步骤为：
将0.094-0.188g分析纯H2L和0.039-0.078g分析纯4,4’-联吡啶溶于10-20mL二次蒸馏水中，调节pH为7后，再加入0.061-0.122g分析纯四水合乙酸锰，置于聚氟四乙烯高压反应釜中，并置于180℃烘箱三天后取出，冷却至室温，打开高压反应釜，底部有浅粉色透明块状晶体即[MnL(4,4’-bpy)0.5]n。通过单晶衍射仪测定[MnL(4,4’-bpy)0.5]n的结构，晶体结构数据见表一,键长键角数据见表二。
本发明具有工艺简单、成本低廉、化学组分易于控制、重复性好并产量高等优点。
附图说明
图1为本发明[MnL(4,4’-bpy)0.5]n所用4-(N,N’-双(4-羧基苄基)氨基)甲苯的结构示意图。
图2为本发明[MnL(4,4’-bpy)0.5]n的单体结构示意图。
图3为本发明[MnL(4,4’-bpy)0.5]n三维堆积示意图。
具体实施方式
实施例1：
本发明涉及的[MnL(4,4’-bpy)0.5]n的单体分子式为：C28H23MnN2O4，分子量为：506.42g/mol,H2L为分析纯4-(N,N’-双(4-羧基苄基)氨基)甲苯，4,4’-bpy为分析纯4,4’-联吡啶。晶体结构数据见表一,键长键角数据见表二。
所述[MnL(4,4’-bpy)0.5]n的合成方法具体步骤为：
将0.094g分析纯H2L和0.039g分析纯4,4’-联吡啶溶于10mL二次蒸馏水中，调节pH为7后，再加入0.061g分析纯四水合乙酸锰，置于聚氟四乙烯高压反应釜中，并置于180℃烘箱三天后取出，冷却至室温，打开高压反应釜，底部有浅粉色透明块状晶体即[MnL(4,4’-bpy)0.5]n。产量0.073g，产率58％。通过单晶衍射仪测定[MnL(4,4’-bpy)0.5]n的结构，晶体结构数据见表一，键长键角数据见表二。
实施例2：
本发明涉及的[MnL(4,4’-bpy)0.5]n的单体分子式为：C28H23MnN2O4，分子量为：506.42g/mol,H2L为分析纯4-(N,N’-双(4-羧基苄基)氨基)甲苯，4,4’-bpy为分析纯4,4’-联吡啶。晶体结构数据见表一,键长键角数据见表二。
所述[MnL(4,4’-bpy)0.5]n的合成方法具体步骤为：
将0.188g分析纯H2L和0.078g分析纯4,4’-联吡啶溶于20mL二次蒸馏水中，调节pH为7后，再加入0.122g分析纯四水合乙酸锰，置于聚氟四乙烯高压反应釜中，并置于180℃烘箱三天后取出，冷却至室温，打开高压反应釜，底部有浅粉色透明块状晶体即[MnL(4,4’-bpy)0.5]n。产量0.152g，产率60％。通过单晶衍射仪测定[MnL(4,4’-bpy)0.5]n的结构，晶体结构数据见表一，键长键角数据见表二。
Claims (1)
1.4-(N,N’-双(4-羧基苄基)氨基)甲苯与4,4’-联吡啶构筑的锰配合物[MnL(4,4’-bpy)0.5]n及合成方法，其特征在于[MnL(4,4’-bpy)0.5]n的单体分子式为：C28H23MnN2O4，分子量为：506.42g/mol,H2L为分析纯4-(N,N’-双(4-羧基苄基)氨基)甲苯，4,4’-bpy为分析纯4,4’-联吡啶。晶体结构数据见表一,键长键角数据见表二；
所述[MnL(4,4’-bpy)0.5]n的合成方法具体步骤为：
将0.094-0.188g分析纯H2L和0.039-0.078g分析纯4,4’-联吡啶溶于10-20mL二次蒸馏水中，调节pH为7后，再加入0.061-0.122g分析纯四水合乙酸锰，置于聚氟四乙烯高压反应釜中，并置于180℃烘箱三天后取出，冷却至室温，打开高压反应釜，底部有浅粉色透明块状晶体即[MnL(4,4’-bpy)0.5]n。通过单晶衍射仪测定[MnL(4,4’-bpy)0.5]n的结构，晶体结构数据见表一,键长键角数据见表二。
表一[MnL(4,4’-bpy)0.5]n的晶体学参数
表二[MnL(4,4’-bpy)0.5]n的部分键长和键角(°)
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- 2017-04-13 CN CN201710242063.1A patent/CN106967123A/zh not_active Withdrawn
Non-Patent Citations (1)
| Title |
|---|
| DONG-YU LV等: "Synthesis, crystal structures, and magnetic properties of two manganese(II) coordination polymers bearing 1,1＇-biphenyl-3,3＇-dicarboxylate ligands", 《TRANSITION MET CHEM》 * |
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