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Method for synthesizing ethyl guaiacol

An ethyl guaiacol and equation technology, applied in chemical instruments and methods, ester reaction preparation of ethers, chemical/physical/physical chemical processes, etc., can solve the problem of large amount of alkylating reagents and catalysts, long reaction time, Low selectivity and other problems, to achieve the effect of less side reactions, short residence time, and improved reaction selectivity

Active Publication Date: 2018-03-20
BEILI CHEM ZHANGJIAGANG
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Problems solved by technology

[0004] The technical problem to be solved in the present invention is: in order to solve the problems of low yield, low selectivity, complex process, large amount of alkylation reagent and catalyst, and high energy consumption in the synthetic method of ethylguaiacol in the prior art , environmental pollution, long reaction time and other problems, a method for synthesizing ethylguaiacol is provided, which has the advantages of high yield, high selectivity, less consumption of alkylating reagents and catalysts, simple process, low energy consumption, No pollution, short reaction time, etc.

Method used

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  • Method for synthesizing ethyl guaiacol
  • Method for synthesizing ethyl guaiacol

Examples

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Embodiment 1

[0028] 71g of catechol was dissolved in 284g of water to obtain a catechol solution, 6.35g of 18-crown-6 ether was dissolved in 317.5g of a mass concentration of 10wt% sodium hydroxide solution to obtain a catalyst solution, and the catechol solution was , catalyst solution and 39.2mL of diethyl carbonate were respectively injected into the continuously heated microreactor from different microchannels according to the flow rates of 89.3mL / min, 81.6mL / min and 10mL / min respectively, and carried out at normal pressure and 50°C. Reaction, control the residence time of the material in the microreactor to 5min, add the mixed solution after the reaction to ethyl acetate for extraction, the ethyl acetate is recovered and recycled, the water phase is adjusted to PH = 2 with hydrochloric acid, and the solid is precipitated, filtered , then rinsed with cold water, dried to obtain ethyl guaiacol, the gas chromatography detection content was 98.4%, the conversion rate of catechol was 95.1%,...

Embodiment 2

[0032] 150g catechol was dissolved in 225g ethanol to obtain catechol solution, and 1.496g 15-crown-5 ether was dissolved in 267g mass concentration to obtain catalyst solution in potassium hydroxide aqueous solution of 28wt%. , catalyst solution and 331mL diethyl carbonate were injected into the continuously heated microreactor from different microchannels at the flow rates of 100mL / min, 71.6mL / min and 89.5mL / min respectively, and the reaction was carried out at normal pressure and 150°C , control the residence time of the material in the microreactor to 0.5min, add the mixed solution after the reaction to extract with ether, recover and recycle the ether, adjust the water phase to PH=3 with sulfuric acid, wait for the solid to precipitate, filter, and then use cold water After rinsing and drying, ethyl guaiacol was obtained. The content detected by gas chromatography was 98.5%, the conversion rate of catechol was 96.5%, and the selectivity of ethyl guaiacol was 88.1%. The NMR...

Embodiment 3

[0036] 71g pyrocatechol was dissolved in 250g benzene to obtain pyrocatechol solution, 10.2g18-crown-6 ether was dissolved in 668g mass concentration to obtain catalyst solution in 15wt% sodium carbonate aqueous solution, pyrocatechol solution, Catalyst solution and 78.5mL diethyl carbonate were injected into the continuously heated microreactor from different microchannels at the flow rates of 47.6mL / min, 100mL / min, and 11.6mL / min respectively, and the reaction was carried out at normal pressure and 120°C , control the residence time of the material in the microreactor to 1min, add the mixed solution after the reaction to extract with ethyl acetate, recover and recycle the ethyl acetate, adjust the water phase to PH=2.2 with phosphoric acid, wait for the solid to precipitate, filter, After rinsing with cold water and drying to obtain ethyl guaiacol, the content detected by gas chromatography is 98.4%, the conversion rate of catechol is 96.5%, the selectivity of ethyl guaiacol ...

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Abstract

The invention relates to a method for synthesizing ethyl guaiacol. The method specifically comprises the following steps: dissolving catechol in a solvent to obtain a catechol solution, dissolving a cyclic crown ether phase transfer catalyst in an inorganic alkali aqueous solution to obtain a catalyst solution, separately injecting the catechol solution, diethyl carbonate and the catalyst solutioninto a continuously-heated micro-reactor from different micro-channels at a flow rate of 10 to 100 mL / min, performing reaction at normal pressure and 50 to 150 DEG C, controlling the retention time of the materials in the micro-reactor at 0.5 to 5 min, and performing the after-treatment on a mixed solution after the reaction is ended, thus obtaining the ethyl guaiacol, wherein a molar ratio of the catechol to the diethyl carbonate to the cyclic crown ether phase transferring catalyst is 1: (0.5 to 2): (0.05 to 0.06). The method for synthesizing the ethyl guaiacol has the advantages of high reaction selectivity, high yield, less consumption of alkylation reagent and catalyst, simple procedure, low energy consumption, no pollution and the like.

Description

technical field [0001] The invention relates to a method for synthesizing ethyl guaiacol, which belongs to the technical field of chemical industry. Background technique [0002] Ethylguaiacol is widely used and is an important organic intermediate, which is widely used in the synthesis of medicine, spices and dyes. In recent years, people have designed a variety of different synthetic routes, which can be summarized into two categories: the first type is to obtain products by dehydrogenating 2-ethoxycyclohexanol as a substrate, but this technology has high energy consumption and reaction The shortcoming that time is long; The second kind is to be reactant with pyrocatechol, and alkyl esters, halogenated alkanes or ethanol etc. are synthesized under conditions such as various catalysts, but there is following technical problem in this route: (1) The selectivity of reaction is low, and yield is low; (2) alkylation reagent and catalyst consumption are large; (3) catalyst need...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/23C07C41/16B01J19/00
CPCB01J19/0093C07C41/16C07C43/23
Inventor 杨巧梅张雯君程文峰任春和徐晓东
Owner BEILI CHEM ZHANGJIAGANG
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