CN103333210B - A kind of [Mn (L) (AcO)] in-situ synthetic method (HOAc) - Google Patents
A kind of [Mn (L) (AcO)] in-situ synthetic method (HOAc) Download PDFInfo
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- CN103333210B CN103333210B CN201310301196.3A CN201310301196A CN103333210B CN 103333210 B CN103333210 B CN 103333210B CN 201310301196 A CN201310301196 A CN 201310301196A CN 103333210 B CN103333210 B CN 103333210B
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- 238000010189 synthetic method Methods 0.000 title claims abstract description 7
- 238000011065 in-situ storage Methods 0.000 title claims description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 title claims description 5
- 229910004373 HOAc Inorganic materials 0.000 title claims description 5
- 239000011572 manganese Substances 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 10
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 10
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 5
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims 1
- 229910052748 manganese Inorganic materials 0.000 claims 1
- 235000021419 vinegar Nutrition 0.000 claims 1
- 239000000052 vinegar Substances 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 6
- KTOXGWMDJYFBKK-UHFFFAOYSA-L manganese(2+);diacetate;dihydrate Chemical compound O.O.[Mn+2].CC([O-])=O.CC([O-])=O KTOXGWMDJYFBKK-UHFFFAOYSA-L 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 3
- 239000000470 constituent Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- YZCKVEUIGOORGS-IGMARMGPSA-N Protium Chemical compound [1H] YZCKVEUIGOORGS-IGMARMGPSA-N 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 150000004696 coordination complex Chemical class 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
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- Plural Heterocyclic Compounds (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses one [Mn (L) (AcO)] synthetic method (HAc). (1) analyze pure 5-acetic acid-1-(6-chloropyridine by 0.15-0.3 gram)-1 hydrogen-pyrazoles-3-methyl acetate and 0.25-0.5 gram analyze pure acetate dihydrate manganese and be dissolved in 10 milliliters of anhydrous acetonitriles; (2) the prepared solution of step (1) is proceeded in the reactor of polytetrafluoroethylene (PTFE), under 80-90 ° of C, react 60-80 hour, be cooled to room temperature, drive still, filter, with ethanol solution washing, obtain monocrystalline level [Mn (L) (AcO)] (HAc). The present invention has overcome the shortcoming of solvent method, has that technique is simple, with low cost, chemical constituent is easy to control, reproducible and output advantages of higher.
Description
Technical field
The present invention relates to [Mn (L) (AcO)] in-situ synthetic method (HAc).
Background technology
There is in recent years original position synthetic technology, at certain condition, by chemical reaction, original position in reaction systemGenerate one or more novel compounds, synthesize by original position, can obtain other synthetic methods and be difficult to the compound obtaining.Nitrogen-containing heterocycle compound is widely used in medicine, agricultural chemicals, pigment, sensitization, dyestuff, energy storage, conduction and biological mould as intermediateIntend material etc. 5-acetic acid-1-(6-chloropyridine)-1 hydrogen-pyrazoles-3-methyl acetate has unique biologically active, taking it as raw materialFor synthetic [Mn (L) (AcO)] (HAc), (H2L=1-(6-chloropyridine)-5-oxygen-4, hydrogen-pyrazoles-3, two hydrogen-1 of 5-, 4-dicarboxylAcid) complex has preferably antibacterial and active anticancer. There is important potential use.
Summary of the invention
Object of the present invention is exactly to be synthetic application nitrogen-containing heterocycle compound 5-acetic acid-1-(6-chloropyridine more widely)-1The transient metal complex of hydrogen-pyrazoles-3-methyl acetate, utilizes solvent thermal process and original position synthetic technology to synthesize [Mn (L)(AcO)] in-situ synthetic method (HAc).
Concrete steps are:
(1) analyze pure 5-acetic acid-1-(6-chloropyridine by 0.15-0.3 gram)-1 hydrogen-pyrazoles-3-methyl acetate and 0.25-Analyzing pure acetate dihydrate manganese for 0.5 gram is dissolved in 10 milliliters of anhydrous acetonitriles.
(2) the prepared solution of step (1) is proceeded in the reactor of polytetrafluoroethylene (PTFE), under 80-90 ° of C, react 60-80Hour, be cooled to room temperature, drive still, filter, with ethanol solution washing, obtain monocrystalline level [Mn (L) is (AcO)] (HAc).
The present invention has overcome the shortcoming of solvent method, has that technique is simple, with low cost, chemical constituent is easy to control, repeatProperty well and output advantages of higher.
Brief description of the drawings
Fig. 1 is the invention process figure.
Fig. 2 is the part H after generation reaction in-situ of the present invention2L molecular structure.
Fig. 3 is the present invention's [Mn (L) (AcO)] structure chart (HAc).
Detailed description of the invention
Embodiment 1:
(1) analyze pure 5-acetic acid-1-(6-chloropyridine by 0.15 gram)-1 hydrogen-pyrazoles-3-methyl acetate and 0.25 gram of analysisPure acetate dihydrate manganese is dissolved in 10 milliliters of anhydrous acetonitriles.
(2) the prepared solution of step (1) is proceeded in the reactor of polytetrafluoroethylene (PTFE), under 80 ° of C, reacts 60 hours,Be cooled to room temperature, drive still, filter, with ethanol solution washing, obtain monocrystalline level [MnL (AcO)] (HAc).
Embodiment 2:
(1) analyze pure 5-acetic acid-1-(6-chloropyridine by 0.3 gram)-1 hydrogen-pyrazoles-3-methyl acetate and 0.5 gram of analysisPure acetate dihydrate manganese is dissolved in 15 milliliters of anhydrous acetonitriles.
(2) the prepared solution of step (1) is proceeded in the reactor of polytetrafluoroethylene (PTFE), under 90 ° of C, reacts 72 hours,Be cooled to room temperature, drive still, filter, with ethanol solution washing, obtain monocrystalline level [Mn (L) (AcO)] (HAc).
Claims (1)
1. [Mn (L) is (AcO)] in-situ synthetic method (HOAc), is characterized in that concrete steps are:
(1) by pure 0.15-0.3 gram of analysisWith the 0.25-0.5 gram of pure two water vinegar of analysisAcid manganese is dissolved in 10 milliliters of anhydrous acetonitriles;
(2) the prepared solution of step (1) is proceeded in the reactor of polytetrafluoroethylene (PTFE), under 80-90 ° of C, react 60-80 littleTime, be cooled to room temperature, drive still, filter, with ethanol solution washing, obtain [Mn (L) is (AcO)] (HOAc);
Described [Mn (L) (AcO)] be middle part H (HOAc)2L molecular structure is:
。
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310301196.3A CN103333210B (en) | 2013-07-18 | 2013-07-18 | A kind of [Mn (L) (AcO)] in-situ synthetic method (HOAc) |
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| CN201310301196.3A CN103333210B (en) | 2013-07-18 | 2013-07-18 | A kind of [Mn (L) (AcO)] in-situ synthetic method (HOAc) |
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| CN103333210A CN103333210A (en) | 2013-10-02 |
| CN103333210B true CN103333210B (en) | 2016-05-18 |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106397487A (en) * | 2016-09-13 | 2017-02-15 | 桂林理工大学 | Complex [Mn2(HL<1>)2(<mu>2-Cl)2(Cl)2] and application of same to preparation of anti-cancer drug |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1519000A (en) * | 1974-09-05 | 1978-07-26 | Ciba Geigy Ag | Complexes of bis-hydrazones and a process for their manufacture |
| CN102426894A (en) * | 2011-09-23 | 2012-04-25 | 桂林理工大学 | Preparation method for monomolecular magnet [Co4(hmb)4(mu3-OMe)4(MeOH)4] |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB9708487D0 (en) * | 1997-04-25 | 1997-06-18 | Bp Chem Int Ltd | Novel catalysts for olefin polymerisation |
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2013
- 2013-07-18 CN CN201310301196.3A patent/CN103333210B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1519000A (en) * | 1974-09-05 | 1978-07-26 | Ciba Geigy Ag | Complexes of bis-hydrazones and a process for their manufacture |
| CN102426894A (en) * | 2011-09-23 | 2012-04-25 | 桂林理工大学 | Preparation method for monomolecular magnet [Co4(hmb)4(mu3-OMe)4(MeOH)4] |
Non-Patent Citations (3)
| Title |
|---|
| Ni(Ⅱ)–牛磺酸缩水杨醛席夫碱•2,2´-联吡啶三元配合物的合成及晶体结构;蒋毅民等，;《结 构 化 学》;20030131;第22卷(第1期);第89-92页 * |
| Synthesis, crystal structure, computational study of 1-(6-chloro-pyridin-2-yl)-5-hydroxy-1H-pyrazole-3-carboxylic acid methyl ester and its 5-acetoxy analogs;Li-Qun Shen等，;《Journal of Molecular Structure》;20120404;第1021卷;第167-173页，尤其是168页方案2化合物2 * |
| Triaqua[2-(2-pyridylmethyleneamino)ethanesulfonato-κ3N,Nˊ,O]nickel(II) perchlorate monohydrate;Jia-Ming Li等，;《Acta Cryst.》;20061231;第m447–m449页 * |
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Effective date of registration: 20201222 Address after: 11 / F, Jingang building, south of Lianyungang Road, Sheyang Economic Development Zone, Sheyang County, Yancheng City, Jiangsu Province 224300 Patentee after: Li Zaigao Address before: 541004 the Guangxi Zhuang Autonomous Region Guilin Construction Road No. 12 Patentee before: GUILIN University OF TECHNOLOGY |
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Effective date of registration: 20221226 Address after: Room 707, Administrative Committee of Tancheng Economic Development Zone, Linyi City, Shandong Province, 276100 Patentee after: Tancheng Economic Development Zone Pharmaceutical Development Co.,Ltd. Address before: 11 / F, Jingang building, south of Lianyungang Road, Sheyang Economic Development Zone, Sheyang County, Yancheng City, Jiangsu Province 224300 Patentee before: Li Zaigao |