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Synthesizing method for 1,2-dimethoxy benzene

A technology of phthalate and a synthesis method, which is applied in the directions of ether preparation, ester reaction preparation of ether, organic chemistry, etc., can solve the problems of increased production cost, cumbersome treatment process, human harm from toluene, etc., and achieves increased cost and simple operation. , The effect of concise production process

Inactive Publication Date: 2013-01-02
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The methyl chloride method of report adopts water and toluene as solvent at present, utilizes phase-transfer catalyst to promote the carrying out of reaction, and yield is 90.2%~95.7%, but the use of phase-transfer catalyst and solvent toluene has increased production cost, and toluene and product The separation of toluene and the recycling of toluene make the post-processing process more cumbersome. In addition, the use of toluene is harmful to the human body. When toluene vapor is mixed with air, it will form explosive substances, which poses a safety hazard.

Method used

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  • Synthesizing method for 1,2-dimethoxy benzene
  • Synthesizing method for 1,2-dimethoxy benzene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1, a kind of synthetic method of phthalic dimethyl ether:

[0018] Add 22.0 g (0.2 mol) of catechol, 16 g (0.4 mol) of sodium hydroxide, and 130 ml of water into a high-pressure reaction kettle with a stirring temperature measuring device, and close the lid of the kettle. use N 2 After checking for leaks and replacing the air several times, 20.2 g (0.4 mol) of methyl chloride was added, the temperature was raised to 50° C., and the pressure was 0.3 MPa. Keep the temperature and pressure for 4h and finish the reaction.

[0019] The reaction solution was left to separate liquids to obtain the lower oil phase, and the atmospheric pressure intermittent distillation was carried out to collect fractions at 216.5-217.7°C to obtain 24.8g of the product with a yield of 90.0% and a purity of 99%. The structure of the obtained product was characterized by infrared spectroscopy. .

Embodiment 2

[0020] Embodiment 2, a kind of synthetic method of phthalic dimethyl ether:

[0021] Add 22.0 g (0.2 mol) of catechol, 20 g (0.5 mol) of sodium hydroxide, and 150 ml of water into a high-pressure reaction kettle with a stirring temperature measuring device, and close the lid of the kettle. use N 2 After checking for leaks and replacing the air several times, 25.2 g (0.5 mol) of methyl chloride was added, the temperature was raised to 60° C., and the pressure was 0.38 MPa. Keep the temperature and pressure for 6h and then finish the reaction.

[0022] The reaction solution was left to separate liquids to obtain the lower oil phase, which was subjected to batch rectification at atmospheric pressure, and the fraction at 216.5-217.7°C was collected to obtain 25.5 g of the product with a yield of 92.5% and a purity of 99%. The structure of the obtained product was characterized by infrared spectroscopy. .

Embodiment 3

[0023] Embodiment 3, a kind of synthetic method of phthalic dimethyl ether:

[0024] Add 22.0 g (0.2 mol) of catechol, 24 g (0.6 mol) of sodium hydroxide, and 180 ml of water into a high-pressure reaction kettle with a stirring temperature measuring device, and close the lid of the kettle. use N 2 After checking for leaks and replacing the air several times, 30.3 g (0.6 mol) of methyl chloride was added, the temperature was raised to 80° C., and the pressure was 0.43 MPa. Keep the temperature and pressure to react for 8h and finish the reaction.

[0025] The reaction solution was left to separate liquids to obtain the lower oil phase, and the batch rectification was carried out at atmospheric pressure, and the fraction at 216.5-217.7°C was collected to obtain 26.3g of the product with a yield of 95.2% and a purity of 99%. The structure of the obtained product was characterized by infrared spectroscopy. .

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Abstract

The invention discloses a synthesizing method for 1,2-dimethoxy benzene, which utilizes pyrocatechol, strong base and chloromethane as raw materials and water as solvent to react in a high pressure autoclave; wherein the mol ratio of strong base to pyrocatechol is 2-3:1, the mole ratio of chloromethane to pyrocatechol is 2-3:1, the reaction temperature is 50-100 DEG C, the reaction pressure is 0.3-0.5 MPa, the reaction time is 4-10h, and the 1,2-dimethoxy benzene is obtained through carrying out liquid separating and rectification on reaction liquid. The method of the invention is adopted to synthesize 1,2-dimethoxy benzene, thus having the characteristics of environment friendless, simple process and high yield.

Description

technical field [0001] The invention relates to a method for synthesizing organic compounds, in particular to a method for synthesizing o-phthalylene dimethyl ether. Background technique [0002] Phthalyl ether, also known as veratrole, has the molecular formula C 8 h 10 o 2 , the pure product is a colorless transparent liquid, solid at low temperature, melting point 22-23°C, has a wide range of industrial uses, is an important fine chemical raw material, not only a key intermediate in the synthesis of dimethomorph, but also a It is used as a reagent for detecting lactic acid in blood and measuring glycerin. [0003] According to different raw materials, the current production methods of o-phthalamide mainly include catechol method, guaiacol method and o-haloanisole method. Guaiacol is a monomethylated product of catechol, and the dimethylated product is phthalate. The methylation reaction of catechol is a series of reactions, and the monomethylation reaction requires s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/205C07C41/16
Inventor 陈新志罗虎钱超
Owner ZHEJIANG UNIV
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