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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, etc., can solve problems such as low yield and unsatisfactory yield, and achieve more efficient and mild reaction And the effect of stabilizing and reducing the generation of by-products

Inactive Publication Date: 2007-08-08
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 methylguaiacol 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 A good aqueous sodium hydroxide solution, after the temperature is stable, drips the glyoxylic acid solution prepared by the above-mentioned (1) simultaneously through three pipelines respectively,

[0027] (2) The remaining aqueous sodium hydroxide solution and (3) methyl guaiacol were dropped after 3 hours, and then continued to stir and react for 1 hour under this condition. After the reaction,...

Embodiment 2

[0029] 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

[0031] 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 discloses a making method of 3-methoxy (or 3-ethoxy)-4-hydroxy amygdalic acid, which comprises the following steps: adopting methyl guaiacol or ethyl guaiacol and glyoxylic acid as raw material; setting the molar rate of methyl guaiacol or ethyl guaiacol and sodium hydroxide at 1:1.1:2.2-1:1.2:2.3; using 0.5-5% quaternary amine compound as catalyst under 28+-1 deg.c; stirring; dripping methyl guaiacol or ethyl guaiacol, glyoxylic acid and residual sodium hydroxide in the alkaline solution of catalyst; finishing dripping course within 3h; reacting for 0.5-2h; selecting catalyst from at least one of tetramethyl ammonium hydroxide, tetramethyl ammonium chloride, tetraethyl ammonium chloride or tetramethyl ammonium bromide; improving product receiving rate to 81.28-86.25%.

Description

technical field [0001] The invention relates to a method for preparing 3-methoxy-4-hydroxymandelic acid by using methylguaiacol or ethylguaiacol and glyoxylic acid as raw materials for condensation reaction in an alkaline solution containing a catalyst or 3-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 present, the synthesis of 3-methoxy-4...

Claims

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Application Information

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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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