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Phenylalanine-1-methyl-3-butyl-imidazole amino acid ionic liquid and preparing method thereof

A technology of butylimidazole and phenylalanine, which is applied in the direction of organic chemistry, can solve environmental pollution and other problems, and achieve the effects of improving sensitivity and activity, wide electrochemical window, and good conductivity

Inactive Publication Date: 2007-09-12
LIAONING UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But D.G.Archer et al pointed out in J.Chem.Eng.Data, 50,1484-1491,2005 that commonly used ionic liquids, such as tetrafluoroborate and hexafluorophosphate of imidazole, are easily partially hydrolyzed in water and produce certain A large amount of negative ions F- will also pollute the environment

Method used

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  • Phenylalanine-1-methyl-3-butyl-imidazole amino acid ionic liquid and preparing method thereof
  • Phenylalanine-1-methyl-3-butyl-imidazole amino acid ionic liquid and preparing method thereof
  • Phenylalanine-1-methyl-3-butyl-imidazole amino acid ionic liquid and preparing method thereof

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Embodiment 1

[0035] Raw materials: n-chlorobutane analytically pure

[0036] Purification: Chlorinated n-butane is collected at 78°C in a distillation device to obtain pure product

[0037] N-Methylimidazole analytically pure

[0038] Purification: N-methylimidazole collects fractions at 188.5°C in a distillation device to obtain pure product

[0039] Acetonitrile Analytical grade

[0040] Purification: add calcium chloride to acetonitrile and reflux in the reflux device for about half an hour, then dry to remove most of the water. Then use the distillation device to distill out the acetonitrile, and collect the fraction at 81-82°C. The product is placed in a bottle filled with 3A molecular sieves and stored in a desiccator

[0041] Ethyl acetate Analytical grade

[0042] Purification: ethyl acetate with anhydrous CaCl 2 Drying, followed by distillation, collected 77.1 ° C fraction. The product is placed in a bottle filled with 3A molecular sieves and stored in a desiccator.

[004...

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Abstract

This invention relates to a Phe-1-methyl-3-butyl imidazole amino acid ionic liquid and its preparation method including: chloro normal butane and N-methyl imidazole are heated and flown back to be synthesized to BMIC, acetic acid, ethyl and acetonit rile solution are heated and flown back to filter the BMIC, ions in anion exchange resin are exchanged to synthesize BMIOH, titration is done to BMIOH with HCl to take the BMIOH solution and add it into D-Phe solution to be mixed for 24h in icy water to eliminate the water and dry it for 48h under 80deg.C to be cooled and added with absolute methyl alcohol and acetonit rile solution to be sealed and beated up for 12h acutely, then placed at 0-10deg.C to pick up the un-reacted D-Phe and depress and filter them, rotate and evaporate to eliminate methyl alcohol and acetonit rile and get the product, which is dried under 80deg.C.

Description

technical field [0001] The invention relates to an ionic liquid and a preparation method thereof, in particular to a novel amino acid ionic liquid and a preparation method thereof. Background technique [0002] Thomas, W. reported in Chem.Rev, 99 (8): 2071-2083, 1999, as early as 1914, the first room temperature ionic liquid ethylammonium nitrate ([EtNH 3 ][NO 3 ]) is synthesized. J.S.Wilkes and M.J.Zaworotko reported in J.Chem.Soc., Chem.Commun, 965-966, 1992 that they synthesized an ionic liquid (IL) EMIBF stable to both water and air 4 . Since then, many new and stable ionic liquids have been continuously synthesized, which are called "green solvents" in the 21st century. But D.G.Archer et al pointed out in J.Chem.Eng.Data, 50,1484-1491,2005 that commonly used ionic liquids, such as tetrafluoroborate and hexafluorophosphate of imidazole, are easily partially hydrolyzed in water and produce certain A large amount of negative ions F- will also pollute the environment. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/70
Inventor 关伟李楠佟静杨家振马溪平李法云
Owner LIAONING UNIVERSITY
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