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Synthesis method of tetrahydrofurfuryl ethyl ether

A technology of ethyl tetrahydrofurfuryl ether and tetrahydrofurfuryl ether, which is applied in the field of synthesis of ethyl tetrahydrofurfuryl ether, can solve the problems of endangering the health of operators, high risk, and environmental pollution, and achieve the elimination of Risk factors, less toxic raw materials, and the effect of reducing pollution emissions

Inactive Publication Date: 2012-08-01
XINJIANG KEYUAN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

A large amount of precious metal sodium or sodium hydride and organic solvents are used in industry, which is dangerous and costly, and will cause serious environmental pollution and endanger the health of operators

Method used

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  • Synthesis method of tetrahydrofurfuryl ethyl ether
  • Synthesis method of tetrahydrofurfuryl ethyl ether
  • Synthesis method of tetrahydrofurfuryl ethyl ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Embodiment 1, synthetic ethyl tetrahydrofurfuryl ether

[0017] In a 500ML reactor, add 102g of tetrahydrofurfuryl alcohol, 0.5mol of diethyl carbonate, and 1mol of potassium hydroxide, react under stirring, control the reaction temperature at 5°C, and finish the reaction after reacting for 9 hours. For the product, the fraction at 150°C-160°C was collected to obtain 98g of the product.

[0018] Adopt Bruker AVANCE DRX 400MHz nuclear magnetic resonance spectrometer to measure product, solvent is deuterated chloroform; Its nuclear magnetic spectrum and resonance peak assignment are as table 1 and figure 1 Shown:

[0019] Table 1. ETE's 1 H-NMR formant assignment

[0020]

[0021] The structure of the product was analyzed by a Nicolet 20DXB FT-IR infrared chromatograph, and the composition and purity of the reaction product were analyzed by a Shimadzu GC-14A gas chromatograph. Chromatographic column: 30m×0.32mm PEG-20M capillary column; column temperature: 40°C / 3 m...

Embodiment 2

[0026] Embodiment 2, synthetic ethyl tetrahydrofurfuryl ether

[0027] In a 500ML reactor, add 102g of tetrahydrofurfuryl alcohol, 0.6mol of diethyl carbonate, and 1mol of sodium hydroxide, react under stirring, control the reaction temperature at 5°C, and finish the reaction after 9 hours of reaction. For the product, the fraction at 150°C-160°C was collected to obtain 96g of the product.

[0028] Adopt Bruker AVANCE DRX 400MHz nuclear magnetic resonance spectrometer to measure product, solvent is deuterated chloroform; Its nuclear magnetic spectrum resonant peak belongs as in Table 2:

[0029] Table 2. ETE's 1 H-NMR formant assignment

[0030]

[0031] The structure of the product was analyzed by a Nicolet 20DXB FT-IR infrared chromatograph, and the composition and purity of the reaction product were analyzed by a Shimadzu GC-14A gas chromatograph. Chromatographic column: 30m×0.32mm PEG-20M capillary column; column temperature: 40°C / 3 minutes to 100°C / 7 minutes; heatin...

Embodiment 3

[0036] Embodiment 3, synthetic ethyl tetrahydrofurfuryl ether

[0037] In a 500ML reactor, add 102g tetrahydrofurfuryl alcohol, 0.6mol diethyl carbonate, and 1mol sodium carbonate, react under stirring, control the reaction temperature at 5°C, and finish the reaction after reacting for 9 hours, and distill the reaction product at atmospheric pressure , collecting fractions at 150°C-160°C to obtain 103g of the product.

[0038] Adopt Bruker AVANCE DRX 400MHz nuclear magnetic resonance spectrometer to measure product, solvent is deuterated chloroform; Its NMR resonance peak attribution is as shown in table 3:

[0039] Table 3. ETE's 1 H-NMR formant assignment

[0040]

[0041] The structure of the product was analyzed by a Nicolet 20DXB FT-IR infrared chromatograph, and the composition and purity of the reaction product were analyzed by a Shimadzu GC-14A gas chromatograph. Chromatographic column: 30m×0.32mm PEG-20M capillary column; column temperature: 40°C / 3 minutes to 10...

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Abstract

The invention discloses a synthesis method of tetrahydrofurfuryl ethyl ether, which comprises the following steps that: tetrahydrofurfuryl alcohol, diethyl carbonate and alkali or alkaline salt are mixed and react to generate the tetrahydrofurfuryl ethyl ether. The molar ratio of the tetrahydrofurfuryl alcohol to the diethyl carbonate to the alkali is 1: (0.5 to 2): (1 to 4). The synthesis methodof the tetrahydrofurfuryl ethyl ether of the invention is safe and has low cost and little pollution.

Description

technical field [0001] The invention relates to a synthesis method of ethyl tetrahydrofurfuryl ether. Background technique [0002] The structure of ethyl tetrahydrofurfuryl ether is an asymmetric structure. The classic asymmetric ether synthesis method is the Williamson synthesis method, which uses halogenated hydrocarbons and sodium alkoxides to synthesize ethers of different hydrocarbon groups through substitution reactions. Most of this kind of reaction adopts anhydrous system. First, metal sodium or sodium hydride is used to convert alcohol into sodium alkoxide, and then the corresponding haloalkane is added to the reaction system. The reaction conditions are relatively harsh and the operation is relatively dangerous. A large amount of precious metal sodium or sodium hydride and organic solvents are used in industry, which is dangerous and costly, and will cause serious environmental pollution and endanger the health of operators. Contents of the invention [0003] T...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/12
Inventor 于荣王毅
Owner XINJIANG KEYUAN CHEM
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