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Continuous coenzyme Q0 producing pipeline process

A pipeline and coenzyme technology, applied in organic chemistry, quinone oxide preparation, etc., can solve problems such as unfavorable safety production, high heat, and unstable process

Inactive Publication Date: 2007-03-21
KUNMING TONGFA IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] According to literature reports, the method of synthesizing 2,3-dimethoxy-5-methyl-1,4-benzoquinone from p-cresol through bromination, methylation, peroxide oxidation and other steps has been patented report, but in the existing method, the methylation reaction time is too long, the peroxide oxidation yield is low, the reaction temperature fluctuates relatively greatly, is not easy to control, affects the yield and quality of the reaction, and the process is unstable
[0005] On the other hand, oxidation with peroxide in the reaction, the reaction releases heat quickly, and the heat is relatively large. There is danger when the concentration of peroxide is high, and safety production is not used.
[0006] The patent of publication number CN86100772 provides a kind of synthetic coenzyme Q 0 The method, this method also uses peroxide as oxidant, improves the yield through process improvement, but there are still problems in reaction control, which is not conducive to industrial production
[0007] Japanese patent (Japanese Patent Application No. 54-106440) describes the use of 60% H 2 o 2 Preparation of coenzyme Q by direct oxidation of 3,4,5-trimethoxytoluene at 0°C 0 , which uses trifluoroacetic acid as a catalyst, the concentration of peroxide in the reaction is relatively high, and there are problems in scale-up production

Method used

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Embodiment Construction

[0026] Implementation column 1

[0027] Add 10kg of 3,4,5-trimethoxytoluene to a 100L glass-lined kettle, 125g of catalyst phosphomolybdic acid, add 12L of formic acid and stir to dissolve completely, and the feed liquid is pumped through a flow pump and hydrogen peroxide at a flow ratio of 4:1. Mix the materials in the pipeline reaction mixer, and the mixed feed liquid enters the pipeline reactor for reaction. The heating section is heated at a water bath temperature of 80°C, and the cooling section is cooled at a water bath temperature of 3°C. The pipe length of the coil heating section is 60m, and the heating section and The length ratio of the cooling and cooling section is 2:1, and the passing speed is 0.2m / s. After the feed liquid comes out of the nozzle, the reaction is completed, and it enters a continuous adding Na 2 CO 3 neutralized in a solid-liquid mixer, Na 2 CO 3 The feed rate is 0.7kg / min. After neutralization, the feed liquid is pumped into a countercurrent ...

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Abstract

The continuous coenzyme Q10 producing pipeline process includes mixing the material 3, 4, 5-trimethoxy toluene and catalyst phosphomolybdic acid, dissolving in formic acid, pumping the formic acid solution and oxidant H2O2 with variable delivery pump to mixer for mixing, reaction in a pipeline reactor, adding Na2CO3 continuously to the reacted liquid, neutralizing in a solid-liquid mixer, continuous extraction of the neutralized liquid in a countercurrent extracting tower, concentrating the extracted liquid in a high efficiency concentrator to eliminate partial solvent, crystallizing the concentrated liquid in a crystallizer through stirring and lower temperature, and filtering to obtain coenzyme Q10. The process has the main features of short production period, easy control of reaction temperature, low cost, continuous reaction, great output and suitability for industrial production.

Description

technical field [0001] The invention relates to the technical field of medicinal chemistry. Specifically relate to a pipelined continuous production of coenzyme Q 0 Methods. Background technique [0002] coenzyme Q 0 The chemical name is 2,3-dimethoxy-5-methyl-1,4 benzoquinone, and the molecular formula is C 9 h 10 o 1 . [0003] coenzyme Q 0 Synthetic coenzyme Q 10 and other important intermediates of quinone compounds, such as coenzyme Q 10 , idebenone, etc., use p-cresol as raw material to synthesize 3,4,5-trimethoxytoluene through bromination, methoxylation, and hydroxymethylation, and then oxidize to synthesize coenzyme Q 0 . [0004] According to literature reports, the method of synthesizing 2,3-dimethoxy-5-methyl-1,4-benzoquinone from p-cresol through bromination, methylation, peroxide oxidation and other steps has been patented report, but in the existing method, the methylation reaction time is too long, the peroxide oxidation yield is low, the reaction ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C50/28C07C46/02
Inventor 王国平骆红成申醒朱锡英符涛
Owner KUNMING TONGFA IND