Method of synthesizing aromatic ether without solvent

A chemical synthesis, solvent-free technology, applied in the direction of ether preparation, organic chemistry, etc., can solve the problems of inability to separate, good water solubility and loss of sodium bromide, and achieve the effects of easy industrial production, accelerated reaction speed, and improved quality

Inactive Publication Date: 2007-02-14
JIAXING UNIV
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  • Description
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Problems solved by technology

Although this method does not use organic solvents and omits the solvent rectification recovery process, the use of water as a solvent has brought about the problem of wastewater ...

Method used

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  • Method of synthesizing aromatic ether without solvent
  • Method of synthesizing aromatic ether without solvent

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Embodiment 1

[0019] 18.5 g (0.1 mol) of sodium 2,4-dichlorophenolate, 1 g of ionic liquid, and 50 g of 2,4-dichlorophenyl isopropyl ether were added to the reactor. A reflux condenser, a stirring device, a dripping device and a thermometer were installed on the reactor, and the 2,4-dichlorophenyl isopropyl ether was heated and melted, and the temperature rose to above 60 °C. 18.5g of isopropane bromide (0.15mol) was added, and the dropwise addition was completed after 1 hour. The reaction temperature was around 60-120°C, and the reaction was refluxed for 3 hours. After cooling, 30g of 2,4-dichlorophenyl isopropyl ether was discharged. Then 18.5 g of sodium 2,4-dichlorophenolate was added, 18.5 g of isopropane bromide was added dropwise, and the reaction was carried out cyclically. After 15 cycles of feeding reaction, 1 g of ionic liquid was added to continue the reaction. The product ether discharged from the bottom was analyzed by gas chromatography, the purity was 99.5%, and the yield w...

Embodiment 2

[0021] Take 22.8 g (0.1 mol) of sodium 5-nitro-2,4-dichlorophenol and 3 g of ionic liquid, add them into the reactor, and add 50 g of 5-nitro-2,4-dichlorophenyl isopropyl ether. Install a reflux condenser, a stirring device, a dripping device and a thermometer on the reactor, heat and melt 5-nitro-2,4-dichlorophenyl n-propyl ether, the temperature rises to above 60 ° C, and start 14.8g (0.12mol) of n-propane bromide was added dropwise through a dropping funnel, and the dropwise addition was completed after 1 hour. The reaction temperature was around 60-120°C, and the reaction was refluxed for 3 hours. After cooling, 30g was discharged. The above-mentioned cyclic feeding reaction was continued, and after 20 reactions, 1 g of ionic liquid was added to continue the reaction. The product 5-nitro-2,4-dichlorophenyl n-propyl ether discharged from the bottom was analyzed by gas chromatography with a purity of 99% and a yield of 98%.

Embodiment 3

[0023] Take 11.6 g (0.1 mol) of sodium phenolate and 0.5 g of ionic liquid, add them into the reactor, and add 50 g of phenyl isopropyl ether. A reflux condenser, a stirring device, a dripping device and a thermometer were installed on the reactor, heated to melt the phenyl isopropyl ether, the temperature rose above 60°C, and 16g (0.13mol) of bromine was added dropwise through the dropping funnel. Substitute isopropane. After 1 hour, the dropwise addition was completed, the reaction temperature was about 60-120° C., the reaction was refluxed for 3 hours, and 20 g was discharged after cooling. The above-mentioned cyclic feeding reaction was continued, and after 15 reactions, 1 g of ionic liquid was added to continue the reaction. The product was analyzed by gas chromatography with a purity of 98.5% and a yield of 97%.

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Abstract

The no-solvation aromatic ether synthesizing process with sodium phenolate or substituted sodium phenolate as main material includes adding small amount of ionic liquid as catalyst and adding halocarbon for reaction to produce aromatic ether. The product aromatic ether is heated to smelt and added into the reaction system as the solvent. The no-solvation aromatic ether synthesizing process has high reactant concentration, high reaction speed, high product yield up to 90 %, high product purity up to 98 %, no use of other solvent, no sewage draining and environment friendship, and is easy use in industrial production.

Description

technical field [0001] The invention relates to a method for preparing aryl ether, and a method for synthesizing aryl ether without solvent. Background technique [0002] Aromatic ethers such as 2,4-dichlorophenyl isopropyl ether and 5-nitro-2,4-dichlorophenyl isopropyl ether are a class of important organic intermediates. The preparation of such aryl ethers can be carried out in the aqueous phase using phase transfer catalytic synthesis. For example, Chinese Patent No. 200410084425.1 describes a method for synthesizing aromatic ethers with water as a solvent under phase transfer catalysis. The catalytic synthesis process is carried out in an aqueous phase, and the product has a purity of over 95% and a yield of over 86%. Although this method does not use organic solvents and omits the solvent distillation recovery process, the use of water as a solvent brings about the problem of treatment of production wastewater. Sodium cannot be separated due to its good water solubili...

Claims

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Application Information

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IPC IPC(8): C07C43/225C07C41/01
Inventor 吴建一
Owner JIAXING UNIV
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