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Preparation method for 3,4-methylene dioxy mandelic acid

A technology of methylenedioxybenzene and glycolic acid, which is applied in the direction of organic chemistry, can solve the problems of large equipment investment, high production cost, and equipment corrosion, and achieve low raw material cost, less three wastes, and elimination of energy consumption and three wastes Effect

Inactive Publication Date: 2014-12-10
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above methods are not ideal, either because the equipment investment is large, the production cost is high, or the equipment is seriously corroded, which is easy to cause environmental pollution.

Method used

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  • Preparation method for 3,4-methylene dioxy mandelic acid
  • Preparation method for 3,4-methylene dioxy mandelic acid
  • Preparation method for 3,4-methylene dioxy mandelic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 45 mL of methanol to a 100-ml three-necked flask, and then add 8.5 g of sodium hydroxide into the methanol and stir to dissolve. After 1 h, 5.2 ml (0.05 mol) of methyl dichloroacetate was added dropwise, and the reaction temperature was controlled at 75°C under continuous microwave radiation heating for 7.5 h to obtain a white opaque solution, and the solid was filtered out. Wash the filter cake with an appropriate amount of methanol, and combine the filtrates. Distill methanol in a constant temperature water bath at 45°C, then add 50% sulfuric acid solution to adjust the pH to 6-8, freeze overnight, filter to desalinate, add 50% sulfuric acid solution to the prepared filtrate to adjust the pH to 2-3, Add 5ml of water and reflux for 3h to obtain 40% glyoxylic acid aqueous solution. The yield is 84.60%.

Embodiment 2-3

[0024] In Example 2-3, the reaction was carried out in the same manner as in Example 1 except for changing the type of base used, the amount of base added, and the amount of methanol added, and the results are shown in the table below.

[0025]

Embodiment 4-7

[0027] In Examples 4-7, except changing the amount of alkali (NaOH), reaction temperature and time, and constant temperature water bath temperature, the reaction was carried out in the same manner as in Example 1, and the results are shown in the table below.

[0028]

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Abstract

The invention relates to a preparation method for a heliotropin midbody such as 3,4-methylene dioxy mandelic acid through microwave radiation. The preparation method comprises the following steps: taking methyl dichloroacetate as a raw material, and reacting with sodium hydroxide or methanol solution of potassium hydroxide under microwave radiation to obtain glyoxylic acid water solution; then reacting the obtained glyoxylic acid water solution with 1,2-methylenedioxybenxene under microwave radiation to prepare 3,4-methylene dioxy mandelic acid finally. Through the application of microwave, under the condition that the reaction time is greatly reduced, the yield of 3,4-methylene dioxy mandelic acid is improved.

Description

technical field [0001] The invention relates to a preparation method of glyoxylic acid and 3,4-methylenedioxymandelic acid. Background technique [0002] Glyoxylic acid, molecular formula C 2 h 2 o 3 , alias formaldehyde formic acid, is the simplest keto acid, has the properties of aldehyde and acid, usually distributed in the body fluids of immature fruits and some animal tissues, and is widely used in the synthesis of varnish raw materials, spices, medicines, dyes, plastics, The intermediate of industrial chemicals can also be used in the production of oral penicillin, jasmonal, vanillin, and allantoin and other products. At present, the preparation methods of glyoxylic acid mainly include glyoxal nitric acid oxidation method, maleic acid ozone oxidation method, dichloroacetic acid hydrolysis oxidation method, oxalic acid electrolytic reduction method, etc. But above-mentioned these methods are not ideal, either equipment investment is big, and production cost is high,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/60
CPCC07D317/60
Inventor 李福祥牛谦熊小晋薛达薛建伟吕志平
Owner TAIYUAN UNIV OF TECH
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