CN109503855A - Polymer 4- (bis- (4- carboxybenzyl) amino of N, N ' -) benzene sulfonic acid manganese and synthetic method - Google Patents
Polymer 4- (bis- (4- carboxybenzyl) amino of N, N ' -) benzene sulfonic acid manganese and synthetic method Download PDFInfo
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- CN109503855A CN109503855A CN201811649860.2A CN201811649860A CN109503855A CN 109503855 A CN109503855 A CN 109503855A CN 201811649860 A CN201811649860 A CN 201811649860A CN 109503855 A CN109503855 A CN 109503855A
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- dpa
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- carboxybenzyl
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- -1 bis- (4- carboxybenzyl) amino Chemical group 0.000 title claims abstract description 16
- 238000010189 synthetic method Methods 0.000 title claims abstract description 8
- 229920000642 polymer Polymers 0.000 title claims abstract description 6
- KCYQEETVXAKDNH-UHFFFAOYSA-N benzenesulfonic acid;manganese Chemical compound [Mn].OS(=O)(=O)C1=CC=CC=C1 KCYQEETVXAKDNH-UHFFFAOYSA-N 0.000 title abstract description 5
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical group CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 16
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical group CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000013078 crystal Substances 0.000 claims abstract description 14
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229940092714 benzenesulfonic acid Drugs 0.000 claims abstract description 7
- ICSNLGPSRYBMBD-UHFFFAOYSA-N 2-aminopyridine Chemical compound NC1=CC=CC=N1 ICSNLGPSRYBMBD-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000178 monomer Substances 0.000 claims abstract description 6
- 239000012153 distilled water Substances 0.000 claims abstract description 5
- 239000011259 mixed solution Substances 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 8
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 4
- 239000011572 manganese Substances 0.000 abstract description 28
- 238000004458 analytical method Methods 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 3
- 239000000470 constituent Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- ATHHXGZTWNVVOU-UHFFFAOYSA-N N-methylformamide Chemical compound CNC=O ATHHXGZTWNVVOU-UHFFFAOYSA-N 0.000 description 4
- 239000003446 ligand Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 125000004429 atom Chemical group 0.000 description 2
- 239000013256 coordination polymer Substances 0.000 description 2
- 229920001795 coordination polymer Polymers 0.000 description 2
- 238000009825 accumulation Methods 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
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 238000004467 single crystal X-ray diffraction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229920001059 synthetic polymer Polymers 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/008—Supramolecular polymers
-
- 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)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of polymer 4- (bis- (4- carboxybenzyl) amino of N, N ' -) benzene sulfonic acid manganese and synthetic methods.The monomer molecule formula of polymer are as follows: C64H54MnN8O14S2, molecular weight are as follows: 1278.21, H3L is to analyze pure 4- (bis- (4- carboxybenzyl) amino of N, N ' -) benzene sulfonic acid, and dpa is to analyze pure 4,4 '-two pyridine amine.Pure H will be analyzed3L and the pure dpa of analysis are dissolved in the mixed solution of secondary distilled water and DMF, and triethylamine is added dropwise and adjusts pH to 6-7, add the pure Mn (CH of analysis3COO)2·4H2O, stirring, reacts 48 hours under 170 DEG C of constant temperatures, is down to room temperature with the rate of 5 DEG C/h, obtain colorless and transparent bulk crystals [Mn (H2L)2(dpa)2]n.Present invention process is simple, low in cost, chemical constituent is easily controllable, reproducible and yield is high.
Description
Technical field
It is [Mn (H the present invention relates to a kind of polymer 4- (bis- (4- carboxybenzyl) amino of N, N ' -) benzene sulfonic acid manganese2L)2
(dpa)2]n(H3L is to analyze pure 4- (bis- (4- carboxybenzyl) amino of N, N ' -) benzene sulfonic acid, and dpa is to analyze pure 4,4 '-two pyridine
Amine) and synthetic method.
Background technique
Coordination polymer (coordination polymer) is a nearly more than ten years Coordinative Chemistry direction with fastest developing speed,
It is one and is related to the multi-disciplinary brand-new research topic such as inorganic chemistry, organic chemistry and Coordinative Chemistry.Have inorganic material concurrently
The flexible characteristic of rigidity and organic material, makes it show huge development potentiality and tempting hair in terms of modern material research
Exhibition prospect.
Summary of the invention
The object of the invention is to be design synthetic polymer 4- (bis- (4- carboxybenzyl) amino of N, N ' -) benzene sulfonic acid manganese,
Utilize solvent structure [Mn (H2L)2(dpa)2]n。
[Mn (H of the present invention2L)2(dpa)2]nMonomer molecule formula are as follows: C64H54MnN8O14S2, molecular weight are as follows:
1278.21 H3L is to analyze pure 4- (bis- (4- carboxybenzyl) amino of N, N ' -) benzene sulfonic acid, and dpa is to analyze pure 4,4 '-two pyridine
Amine.Crystal structural data is shown in Table one, and bond distance's bond angle data are shown in Table two.
One, of table [Mn (H2L)2(dpa)2]nCrystallographic parameter
Two, of table [Mn (H2L)2(dpa)2]nPart bond distanceWith bond angle (°)
[Mn (the H2L)2(dpa)2]nSynthetic method specific steps are as follows:
(1) 0.110-0.220g is analyzed into pure H3L and 0.086-0.172g analyzes pure dpa and is dissolved in 7-14mL secondary distilled water
In the mixed solution for analyzing pure n,N-Dimethylformamide (DMF) with 1-2mL, it is added dropwise and analyzes pure triethylamine adjusting pH to 6-7, then
0.062-0.124g is added and analyzes pure Mn (CH3COO)2·4H2O, continue stirring to solution it is uniform after, be placed in polytetrafluoroethylene (PTFE) height
It presses in reaction kettle, is placed in airtight oven, is reacted 48 hours under 170 DEG C of constant temperatures, room is down to the rate of 5 DEG C/h
Temperature obtains colorless and transparent bulk crystals [Mn (H2L)2(dpa)2]n。
[Mn (H is measured by single crystal diffractometer2L)2(dpa)2]nStructure, crystal structural data is shown in Table one, bond distance's bond angle
Data are shown in Table two.
The present invention has many advantages, such as that simple process, low in cost, chemical constituent is easily controllable, reproducible and yield is high.
Detailed description of the invention
Fig. 1 is the present invention { [Mn (H2L)2(dpa)2]nThe knot of 4- (bis- (4- carboxybenzyl) amino of N, N ' -) benzene sulfonic acid used
Structure schematic diagram.
Fig. 2 is the present invention [Mn (H2L)2(dpa)2]nMonomer structure schematic diagram.
Fig. 3 is the present invention [Mn (H2L)2(dpa)2]nMetallic atom coordination configuration figure.
Fig. 4 is the present invention [Mn (H2L)2(dpa)2]nThree-dimensional accumulation schematic diagram.
Single-crystal X-ray diffraction analysis shows [Mn (H2L)2(dpa)2]nIt is monoclinic system, space group P21/n.It can from Fig. 2
Know, basic building unit includes individual Mn (II) atom, two H2L ligand and two dpa ligands.From the figure 3, it may be seen that Mn
(II) and from four H2The oxygen atom (O1, O1A, O3B, O3C) of L ligand and two nitrogen-atoms on two dpa ligands
(N1, N1A) coordination forms the octoploids structure of the square distortion of hexa-coordinate.
Specific embodiment
Embodiment 1:
[Mn (H of the present invention2L)2(dpa)2]nMonomer molecule formula are as follows: C64H54MnN8O14S2, molecular weight are as follows:
1278.21 H3L is to analyze pure 4- (bis- (4- carboxybenzyl) amino of N, N ' -) benzene sulfonic acid, and dpa is to analyze pure 4,4 '-two pyridine
Amine.Crystal structural data is shown in Table one, and bond distance's bond angle data are shown in Table two.
[Mn (the H2L)2(dpa)2]nSynthetic method specific steps are as follows:
0.110g is analyzed into pure H3L and 0.086g analyzes pure dpa and is dissolved in 7mL secondary distilled water and 1mL analysis pure N, N- bis-
In the mixed solution of methylformamide (DMF), it is added dropwise and analyzes pure triethylamine adjusting pH to 6-7, add 0.062g and analyze pure Mn
(CH3COO)2·4H2O, continue stirring to solution it is uniform after, be placed in polytetrafluoroethylene (PTFE) autoclave, be placed in airtight oven
In, it is reacted 48 hours under 170 DEG C of constant temperatures, room temperature is down to the rate of 5 DEG C/h, obtains colorless and transparent bulk crystals
[Mn(H2L)2(dpa)2]n.Yield 0.213g, yield 65%.[Mn (H is surveyed by single crystal diffractometer2L)2(dpa)2]nStructure, it is brilliant
Body structured data is shown in Table one, and bond distance's bond angle data are shown in Table two.
Embodiment 2:
[Mn (H of the present invention2L)2(dpa)2]nMonomer molecule formula are as follows: C64H54MnN8O14S2, molecular weight are as follows:
1278.21 H3L is to analyze pure 4- (bis- (4- carboxybenzyl) amino of N, N ' -) benzene sulfonic acid, and dpa is to analyze pure 4,4 '-two pyridine
Amine.Crystal structural data is shown in Table one, and bond distance's bond angle data are shown in Table two.
[Mn (the H2L)2(dpa)2]nSynthetic method specific steps are as follows:
0.220g is analyzed into pure H3L and 0.172g analyzes pure dpa and is dissolved in 14mL secondary distilled water and 2mL analysis pure N, N- bis-
In the mixed solution of methylformamide (DMF), it is added dropwise and analyzes pure triethylamine adjusting pH to 6-7, add 0.124g and analyze pure Mn
(CH3COO)2·4H2O, continue stirring to solution it is uniform after, be placed in polytetrafluoroethylene (PTFE) autoclave, be placed in airtight oven
In, it is reacted 48 hours under 170 DEG C of constant temperatures, room temperature is down to the rate of 5 DEG C/h, obtains colorless and transparent bulk crystals
[Mn(H2L)2(dpa)2]n.Yield 0.446g, yield 68%.[Mn (H is measured by single crystal diffractometer2L)2(dpa)2]nStructure,
Crystal structural data is shown in Table one, and bond distance's bond angle data are shown in Table two.
Claims (1)
1. a kind of polymer [Mn (H2L)2(dpa)2]n, it is characterised in that [Mn (H2L)2(dpa)2]nMonomer molecule formula are as follows:
C64H54MnN8O14S2, molecular weight are as follows: 1278.21, H3L is to analyze pure 4- (bis- (4- carboxybenzyl) amino of N, N ' -) benzene sulfonic acid,
Dpa is to analyze pure 4,4 '-two pyridine amine；Crystal structural data is shown in Table one, and bond distance's bond angle data are shown in Table two；
One, of table [Mn (H2L)2(dpa)2]nCrystallographic parameter
Two, of table [Mn (H2L)2(dpa)2]nPart bond distanceWith bond angle (°)
[Mn (the H2L)2(dpa)2]nSynthetic method specific steps are as follows:
(1) 0.110-0.220g is analyzed into pure H3L and 0.086-0.172g analyzes pure dpa and is dissolved in 7-14mL secondary distilled water and 1-
2mL is analyzed in the mixed solution of pure n,N-Dimethylformamide (DMF), is added dropwise and is analyzed pure triethylamine adjusting pH to 6-7, adds
0.062-0.124g analyzes pure Mn (CH3COO)2·4H2O, continue stirring to solution it is uniform after, it is anti-to be placed in polytetrafluoroethylene (PTFE) high pressure
It answers in kettle, is placed in airtight oven, reacted 48 hours under 170 DEG C of constant temperatures, room temperature is down to the rate of 5 DEG C/h, is obtained
To colorless and transparent bulk crystals [Mn (H2L)2(dpa)2]n。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811649860.2A CN109503855A (en) | 2018-12-31 | 2018-12-31 | Polymer 4- (bis- (4- carboxybenzyl) amino of N, N ' -) benzene sulfonic acid manganese and synthetic method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811649860.2A CN109503855A (en) | 2018-12-31 | 2018-12-31 | Polymer 4- (bis- (4- carboxybenzyl) amino of N, N ' -) benzene sulfonic acid manganese and synthetic method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109503855A true CN109503855A (en) | 2019-03-22 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811649860.2A Withdrawn CN109503855A (en) | 2018-12-31 | 2018-12-31 | Polymer 4- (bis- (4- carboxybenzyl) amino of N, N ' -) benzene sulfonic acid manganese and synthetic method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109503855A (en) |
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2018
- 2018-12-31 CN CN201811649860.2A patent/CN109503855A/en not_active Withdrawn
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Application publication date: 20190322 |