O-ethoxyl phenol synthesizing process

A technology of o-ethoxyphenol and synthesis method, applied in the direction of organic chemistry, can solve the problems of high yield, high toxicity of diethyl sulfate, serious environmental pollution, etc., and achieve short process, low one-time investment and low product cost Falling effect

Inactive Publication Date: 2005-12-14
CNPC JILIN CHEM GROUP CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method has high yield and good selectivity; however, diethyl sulfate is highly toxic and pollutes the environment more seriously

Method used

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  • O-ethoxyl phenol synthesizing process

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Experimental program
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Effect test

Embodiment 1

[0027] In the autoclave, add toluene 800g, water 480g, start stirring, turn on the autoclave shaft cooling water, then add catechol 176g, sodium carbonate 8g, tetrabutylammonium bromide 12g, solid sodium hydroxide 89.6g, chlorine 165g of ethane, after sealing the cover, fill it with nitrogen to 1.0Mpa, keep it for 2 minutes, check for air leakage, if there is no air leakage, release the pressure. Start to heat up, keep at 130-139°C and 0.1-1.1MPa pressure for 2 hours, cool down to room temperature after the reaction, open the autoclave after pressure relief, pour the feed liquid into the separatory funnel, and separate the liquids. Add hydrochloric acid to the water phase to adjust the pH value to 5-6. After fully extracting with toluene, combine the oil phases. The oil layer is distilled under normal pressure and under reduced pressure to obtain o-ethoxyphenol products with a purity ≥ 98.0%. The solvent recovered by distillation is recycled. The obtained product was weighed...

Embodiment 2

[0031] In the autoclave, add 800g of toluene, 500g of water, start stirring, turn on the cooling water of the autoclave shaft, then add 220g of catechol, 20g of sodium carbonate, 9g of tetraethylammonium bromide, 104g of solid alkali, and 180g of ethyl chloride , After sealing the cover, fill nitrogen to 1.0Mpa, keep it for 2 minutes, check for air leakage, if there is no air leakage, release the pressure. Start to heat up, keep at 120-130°C and 0.1-1.1MPa pressure for 4 hours, cool down to room temperature after the reaction is over, open the autoclave after pressure relief, pour the feed liquid into the separatory funnel, and separate the liquids. Add hydrochloric acid to the water phase to adjust the pH value to 5-6. After fully extracting with toluene, combine the oil phases. The oil layer is distilled under normal pressure and under reduced pressure to obtain o-ethoxyphenol products with a purity ≥ 98.0%. The solvent recovered by distillation is recycled. The obtained p...

Embodiment 3

[0033] In the autoclave, add 500g of toluene, 350g of water, start stirring, turn on the cooling water of the autoclave shaft, then add 220g of catechol, 60g of sodium carbonate, 2g of tetramethylammonium bromide, 80g of solid alkali, and 130g of ethyl chloride , After sealing the cover, fill nitrogen to 1.0Mpa, keep it for 2 minutes, check for air leakage, if there is no air leakage, release the pressure. Start to heat up, keep at 100-120°C and 0.2-1.0MPa pressure for 6 hours, cool down to room temperature after the reaction is over, open the autoclave after the pressure is released, pour the feed liquid into the separatory funnel, and separate the liquids. Add hydrochloric acid to the water phase to adjust the pH value to 5-6. After fully extracting with toluene, combine the oil phases. The oil layer is distilled under normal pressure and under reduced pressure to obtain o-ethoxyphenol products with a purity ≥ 98.0%. The solvent recovered by distillation is recycled. The o...

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Abstract

The o-ethoxyl phenol synthesizing process with catechol and ethyl chloride as material includes the following steps: adding toluene and water into high pressure reactor, starting stirrer and water cooling the shaft of the high pressure reactor; adding catechol, sodium carbonate, alkyl amine bromide catalyst, solid sodium hydroxide, ethyl chloride in required amount successively; sealing, heating and maintaining at 100-139 deg.c and 0.1-1.1 MPa for 2-6 hr. The weight proportion among catechol, sodium hydroxide, sodium carbonate, ethyl chloride, alkyl amine bromide, water and toluene is 1 to 0.364-0.509 to 0.045-0.273 to 0.591-0.938 to 0.0091-0.0682 to 1.591-2.730 to 1.820-4.545. The present invention has yield of 86 %, and compared with other process, the present invention has lowered product cost, less sewage exhaust, low sewage COD, short technological process and less investment.

Description

technical field [0001] The invention relates to a method for synthesizing o-ethoxyphenol, in particular to a method for synthesizing o-ethoxyphenol by using catechol and ethyl chloride as raw materials in the presence of a phase transfer catalyst. Background technique [0002] O-ethoxyphenol, also known as o-hydroxyphenethyl ether and ethyl guaiacol, is an important raw material for the synthesis of ethyl vanillin and an indispensable intermediate in the pharmaceutical industry. At present, there are two main methods for synthesizing o-ethoxyphenol at home and abroad, i.e. o-aminophenethyl ether method and catechol method: [0003] 1. O-aminophenethyl ether method: [0004] The method is that in the presence of sulfuric acid, diazotization reaction is carried out with sodium nitrite in the presence of sulfuric acid, and then hydrolyzed under the action of copper sulfate to generate o-ethoxyphenol. The process was applied earlier and widely, the pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/253
Inventor 郭双龙苑冰盛光陈继新王芳石占崇阎圣刚黄晓东
Owner CNPC JILIN CHEM GROUP CORP
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