1, 4-dimethyl-1-alkyl piperazine ionic liquid as well as preparation method and applications thereof

A technology of alkylpiperazine and ionic liquid, applied in the field of organic synthesis, can solve problems such as long preparation period, and achieve the effects of short preparation period, high yield and low viscosity

Inactive Publication Date: 2014-04-09
ZHEJIANG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation cycle of this preparation method is too long, and the purity of the product is not involved

Method used

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  • 1, 4-dimethyl-1-alkyl piperazine ionic liquid as well as preparation method and applications thereof
  • 1, 4-dimethyl-1-alkyl piperazine ionic liquid as well as preparation method and applications thereof
  • 1, 4-dimethyl-1-alkyl piperazine ionic liquid as well as preparation method and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Example 1: Preparation of 1,4-dimethyl-1-ethylpiperazine ionic liquid chloride

[0034] In a 500mL three-necked flask equipped with a dropping funnel, reflux condenser and nitrogen balloon, add 1.3mol 1-chloroethane and 100mL ethyl acetate, and add 1mol 1,4-dimethylpiperazine and 100mL to the dropping funnel The ethyl acetate was slowly dropped into the ethyl acetate solution of 1-chloroethane, stirred and reacted at 80°C for 48 hours, cooled to room temperature, filtered, and the white solid obtained was washed with ethyl acetate and dried under vacuum at 40°C. The 1,4-dimethyl-1-ethylpiperazine chloride ionic liquid was obtained with a purity of 99% and a yield of 80%.

Embodiment 2

[0035] Example 2: Preparation of 1,4-dimethyl-1-propylpiperazine iodide ionic liquid

[0036] In a 500mL three-necked flask equipped with a dropping funnel, reflux condenser and nitrogen balloon, add 1.2mol 1-iodopropane and 100mL ethyl acetate, and add 1mol 1,4-dimethylpiperazine and 100mL acetic acid to the dropping funnel The ethyl ester was slowly dropped into the ethyl acetate solution of 1-iodopropane, stirred and reacted at 30°C for 12 hours, cooled to room temperature, filtered, and the white solid obtained was washed with ethyl acetate and dried under vacuum at 40°C to obtain iodine 1,4-Dimethyl-1-propylpiperazine ionic liquid, purity 99%, yield 86%.

Embodiment 3

[0037] Example 3: Preparation of 1,4-dimethyl-1-butylpiperazine iodide ionic liquid

[0038] In a 500mL three-necked flask equipped with a dropping funnel, a reflux condenser and a nitrogen balloon, add 1.1mol 1-iodobutane and 100mL ethyl acetate, and add 1mol 1,4-dimethylpiperazine and 100mL to the dropping funnel The ethyl acetate was slowly dropped into the ethyl acetate solution of 1-iodobutane, stirred and reacted at 40°C for 24 hours, cooled to room temperature, filtered, and the white solid obtained was washed with ethyl acetate and dried under vacuum at 50°C The 1,4-dimethyl-1-butylpiperazine iodide ionic liquid was obtained with a purity of 99% and a yield of 91%.

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PUM

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Abstract

The invention discloses a 1, 4-dimethyl-1-alkyl piperazine ionic liquid. The chemical structural general formula of the 1, 4-dimethyl-1-alkyl piperazine ionic liquid is as shown in the specification, wherein the R is straight-chain alkyl of C1-C10; the negative ion Y<-1> is Cl<-1>, Br<-1>, I<-1>, C4F9SO3<-1>, C4H9OSO3<-1>, C6H13OSO3<-1>, C8H17OSO3<-1>, (CF3SO2)2N <-1>, (CF3SO2)3C<-1>, (C2F5SO2)2N<-1> or (C2F5SO2)3C<-1>. The invention further discloses a preparation method of the 1, 4-dimethyl-1-alkyl piperazine ionic liquid. The preparation method is simple in process and short in preparation cycle and has the advantages that the product yield reaches above 70%, and the product purity can reach above 96%. The invention further discloses the application of the 1, 4-dimethyl-1-alkyl piperazine ionic liquid serving as a gas chromatography stationary phase and the application of the 1, 4-dimethyl-1-alkyl piperazine ionic liquid in sulfur dioxide gas absorption.

Description

Technical field [0001] The invention relates to the field of organic synthesis, in particular to a 1,4-dimethyl-1-alkylpiperazine ionic liquid, a preparation method and application thereof. Background technique [0002] Ionic liquids are generally composed of organic cations and inorganic or organic anions, and are salts that are liquid at or near room temperature. Ionic liquid has the characteristics of low vapor pressure, good thermal and chemical stability, and strong adjustability. It can be used as an excellent green solvent and catalyst, and is widely used in catalytic synthesis, separation technology, electrochemistry, petrochemical industry, etc. field. Ionic liquids are expected to replace traditional organic solvents that are volatile, highly toxic, flammable and explosive, and thus have received extensive attention from academic and industrial circles at home and abroad. [0003] At present, the ionic liquids widely studied and used mainly use imidazole and pyridine as...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D295/023C07D295/037C07C305/06C07C303/24C07C311/48C07C303/40C07C309/06C07C303/32B01J20/292B01D53/14
CPCB01D53/1493B01D2252/20447B01J20/292C07D295/023C07D295/037
Inventor 陆晓星曹琦方文军郭永胜许莉胡申林
Owner ZHEJIANG UNIV
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