Micro-wave synthetic method for preparing methyl salicylate

A technology for methyl salicylate and microwave synthesis, which is applied in the preparation of carboxylate esters, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of cumbersome post-processing, complicated equipment, and long reaction time, and achieve the goal of reaction time The effect of shortening, simple equipment and low energy consumption

Inactive Publication Date: 2008-07-23
ZHEJIANG UNIVERSITY OF SCIENCE AND TECHNOLOGY
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Problems solved by technology

[0003] In order to overcome the deficiencies of long reaction time, complex equipment and cumbersome post-treatment of the currently known synthetic methods, the purpose of this

Method used

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Examples

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Embodiment 1

[0030] Heat and stir 12.0g salicylic acid and 20.88g anhydrous methanol in a beaker and pour it into a three-neck flask, then place it on the glass round table in the microwave oven, and use a condenser tube to pass through the small round hole on the top of the microwave oven. The two-necked glass tube is docked with the round bottom flask in the microwave oven, slowly add 3.0ml of concentrated sulfuric acid, maintain reflux, set the reaction power to 195 watts, and stop heating after 25 minutes of radiation reaction. After cooling, pour the liquid into a beaker, add distilled water to wash out the oil layer until the upper layer is clear and transparent. Pour it into a separatory funnel and let it stand to separate the lower oil layer. Wash with 20% sodium carbonate solution to pH=7. After adding distilled water, pour it into a separatory funnel, and separate the lower oil layer. Dry over anhydrous magnesium sulfate. After vacuum filtration, the filtrate was distilled und...

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Abstract

The invention discloses a microwave synthetic preparation method for methyl salicylate, which is characterized in that: salicylic acid and methanol are used as raw material and concentrated sulfuric acid is used as catalyst; heating is made for reflux reaction under microwave radiation condition before separating to get salicylic acid methyl ester. The microwave synthetic preparation method for methyl salicylate has the advantages of greatly improving reaction ratio and shortening reaction time and significantly increasing reaction yield compared with normal preparation method for methyl salicylate.

Description

technical field [0001] The invention relates to organic synthesis technology, in particular to a microwave synthesis method for preparing methyl salicylate. Background technique [0002] The scientific name of methyl salicylate is methyl o-hydroxybenzoate, which is a colorless or red oily liquid. Because it is the main component of the distilled oil of wintergreen leaves, it has the spirit of wintergreen, so it is commonly known as wintergreen oil. Methyl salicylate is a chemical product with a wide range of uses, mainly used in edible and cosmetic flavors, such as tuberose, acacia, etc., strawberry, grape, etc. food flavors, and can also be used in insecticides and fungicides , analgesics, solvents and intermediates for glazing agents and coatings, etc. The output of natural wintergreen oil extract is very limited, and industrial preparation of methyl salicylate is mainly used. The main method of industrially synthesizing methyl salicylate at present is: take concentrate...

Claims

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Application Information

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IPC IPC(8): C07C69/84C07C67/08
Inventor 张立庆李菊清
Owner ZHEJIANG UNIVERSITY OF SCIENCE AND TECHNOLOGY
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