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Method of synthesizing 3-methoxy-4-dydroxymandelic acid or 3-ethoxy-4-dydroxymandelic acid by acetaldehyde acid method

A technology of hydroxymandelic acid and glyoxylic acid, applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylate and other directions, can solve problems such as low yield, unsatisfactory yield and the like, achieve mild and stable reaction, The effect of reducing the generation of by-products

Inactive Publication Date: 2009-08-12
CNPC JILIN CHEM GROUP CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Over the years, experts and scholars in some enterprises, institutions and institutions of higher learning have taken improving the yield of vanillin and ethyl vanillin as an important subject for research, but the yield is still not ideal
The method for the synthesis of vanillin and ethyl vanillin by the glyoxylic acid method disclosed at present, the main problem is that the yield is low

Method used

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  • Method of synthesizing 3-methoxy-4-dydroxymandelic acid or 3-ethoxy-4-dydroxymandelic acid by acetaldehyde acid method
  • Method of synthesizing 3-methoxy-4-dydroxymandelic acid or 3-ethoxy-4-dydroxymandelic acid by acetaldehyde acid method
  • Method of synthesizing 3-methoxy-4-dydroxymandelic acid or 3-ethoxy-4-dydroxymandelic acid by acetaldehyde acid method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Weigh 37g of glyoxylic acid and add it to 57g of water, stir well and set aside.

[0024] (2) Weigh 18.8g of sodium hydroxide and add 140g of water to prepare a sodium hydroxide solution for later use.

[0025] (3) Weigh 27 g of guaiacol with a mass content of 99.4% for later use.

[0026] Weigh 110g of water and add it to the condensation kettle equipped with a constant temperature water bath, agitator and thermometer, start stirring, raise the temperature to 28°C, add 0.5g of catalyst A (tetramethylammonium hydroxide), and then add 17g of the above (2) to prepare After the temperature of the good sodium hydroxide aqueous solution is stabilized, the above-mentioned (1) prepared glyoxylic acid solution, (2) the remaining sodium hydroxide aqueous solution and (3) guaiacol are added dropwise through the three pipelines at the same time. Finished, continue to stir reaction 1h under this condition again. After the reaction, take a sample and analyze the content of 3-m...

Embodiment 2

[0028] According to the operating steps of Example 1, catalyst B (tetramethylammonium chloride), catalyst C (tetramethylammonium bromide), catalyst A plus B (by mass, A: B=1: 1), Catalyst A plus C (by mass, A:C=1:1), catalyst B and C (by mass, B:C=1:1), catalyst A plus B plus C (by mass, A:B : C=1: 2: 2), all the other technological conditions remain unchanged with embodiment 1, and test result sees attached table.

Embodiment 3

[0030] According to the operating steps of embodiment 1, except changing the reaction time, all the other processing conditions are identical with embodiment 1, and test result sees the attached table below.

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Abstract

The invention relates to a method for preparing 3-methoxy (or 3-ethoxy)-4-hydroxymandelic acid, which uses guaiacol or ethyl guaiacol and glyoxylic acid as raw materials, and glyoxylic acid , guaiacol or ethyl guaiacol, the molar ratio of sodium hydroxide is 1: 1.1: 2.2~1: 1.2: 2.3, with quaternary ammonium salt compound as catalyst, its consumption is guaiacol or ethyl guaiacol 0.5% to 5% of the mass of the base guaiacol, and the reaction temperature is 28±1°C, and the required amount of guaiacol or ethyl guaiacol, Glyoxylic acid and the remaining sodium hydroxide solution were added dropwise within 3 hours, and then reacted under the conditions for 0.5-2 hours. The quaternary ammonium salt compound catalyst is selected from at least one of tetramethylammonium hydroxide, tetramethylammonium chloride, tetraethylammonium chloride or tetramethylammonium bromide, etc., and its product yield is 81.28 ~86.25%.

Description

technical field [0001] The present invention relates to a method to prepare 3-methoxy-4-hydroxymandelic acid or 3-methoxy-4-hydroxymandelic acid by using guaiacol or ethyl guaiacol and glyoxylic acid as raw materials for condensation reaction in an alkaline solution containing a catalyst - Ethoxy-4-hydroxymandelic acid method. Background technique [0002] 3-methoxy-4-hydroxymandelic acid (3-methoxy-4-hydroxymandelic acid) and 3-ethoxy-4-hydroxymandelic acid (3-ethoxy-4-hydroxymandelic acid ) is an important intermediate for the synthesis of vanillin and ethyl vanillin, and vanillin or ethyl vanillin is a broad-spectrum type of spice that can be used as a fixative, flavoring agent and flavor-changing agent; in addition, it is also a synthetic Important intermediates of medicine, such as: 3-methoxy-4-hydroxymandelic acid is an important intermediate for the preparation of sulfonamide synergist 3,4,5-trimethoxypyrimidine TMP. [0003] According to literature reports, at pres...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/00C07C59/64
Inventor 李耀先魏国峰刘乃青侯淑兰刘长青
Owner CNPC JILIN CHEM GROUP CORP
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