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Preparation method of catalyst for oxidative synthesis of folic acid from 6-R-tetrahydrofolic acid

A technology for oxidative synthesis and tetrahydrofolic acid, applied in the direction of organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problems of poor selectivity of oxidation products and achieve improved oxidation Reaction efficiency, simple recycling and reuse, and simple synthesis process

Pending Publication Date: 2022-02-11
HARBIN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the selectivity of the oxidation products of tetrahydrofolate is extremely poor, and the oxidation products obtained by various oxidants under normal conditions are complex mixtures, including folic acid, dihydrofolate, pterin, p-aminobenzoyl glutamic acid, etc., no Synthetic meaning

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 110

[0017] Example 1. Suspend 10g of SBA-15 molecular sieve in 100ml of chloroform / ethanol (2:1) solution, add 1g of tetraphenylporphyrin, dissolve under stirring, and reflux for 2 hours. 0.6g nickel acetate tetrahydrate and 0.7g manganese acetate tetrahydrate were dissolved in 30ml ethanol / water (5:1) solution. The mixed solution was added into the reaction system, and the reflux reaction was continued for 4 hours. Filter, wash with distilled water for 3 times, and vacuum dry to obtain a supported composite catalyst.

[0018] The effect test of the supported composite catalyst was carried out according to the following steps: 4.6 g of 6-R-tetrahydrofolate was dissolved in 50 ml of water. Adjust the pH value to 7, add 92 mg of the above-mentioned supported composite catalyst, stir at 25 ° C, slowly add 40 ml of hydrogen peroxide with a concentration of 5%, and react for 6 hours. After 6 hours of reaction, TLC monitors that all raw materials are consumed, continue stirring for 60 ...

Embodiment 2

[0019] Embodiment 2. supported composite catalyst is synthesized by the operation process of embodiment 1, just changes the consumption of tetraphenylporphyrin into 0.5g, changes the nickel acetate tetrahydrate consumption into 0.3g, and changes the manganese acetate tetrahydrate consumption into 0.36g , 20ml of ethanol aqueous solution.

[0020] The reaction time in the test result of the supported composite catalyst effect is 12 hours. The product was separated and recrystallized by ethanol to refine 4.0 g of folic acid with a purity of 98.4%. The yield of refined folic acid is 87.7%.

Embodiment 3

[0021] Embodiment 3. supported composite catalyst is synthesized by the operating process of embodiment 1, just changes the consumption of tetraphenylporphyrin into 1.5g, changes the nickel acetate tetrahydrate consumption into 0.9g, and changes the manganese acetate tetrahydrate consumption into 1.1g , 50ml of ethanol aqueous solution.

[0022] The reaction time in the test result of the supported composite catalyst effect is 6 hours. After the product was separated and recrystallized by ethanol, 4.1 g of folic acid was refined, with a purity of 98.5%. The yield of refined folic acid is 89.9%.

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Abstract

The invention mainly relates to a preparation method of a supported composite catalyst for oxidative synthesis of folic acid from 6-R-tetrahydrofolic acid. The preparation method of the supported composite catalyst for oxidative synthesis of folic acid from 6-R-tetrahydrofolic acid comprises the following steps: suspending a certain amount of a SBA-15 molecular sieve in chloroform / ethanol (2: 1) solution accounting for 10 times of the volume of the SBA-15 molecular sieve, adding a certain amount of tetraphenylporphyrin, conducting dissolving while stirring, performing refluxing for 2 hours, adding a certain amount of ethanol / water (5: 1) solution of nickel acetate and manganese acetate, and continuing refluxing for 4 hours; and carrying out filtering, performing washing with distilled water three times, and carrying out drying in vacuum to obtain the supported composite catalyst. The catalyst is used in a reaction for synthesizing folic acid through hydrogen peroxide oxidation of 6-R-tetrahydrofolic acid, and catalytic effect is good. The catalyst accounting for 2% of the weight of the raw material is used, the purity of the refined folic acid product can reach 98.5% or above, and yield is 90% or above.

Description

technical field [0001] The invention relates to a preparation method of a loaded composite catalyst used for oxidatively synthesizing folic acid from 6-R-tetrahydrofolate, and belongs to the technical field of fine chemicals. Background technique [0002] In the process of synthesizing 6-S-5-methyltetrahydrofolate with folic acid as raw material, when folic acid is reduced to 6-R,S-tetrahydrofolate and separated to obtain 6-S-tetrahydrofolate, a large amount of by-products Biologically active 6-R-tetrahydrofolate. Since it has not been found to have other uses, it can only be treated as production waste. The treatment process not only increases the production cost, but also brings about relatively large environmental problems. [0003] In order to solve this problem, an effective method is to obtain folic acid by catalytic oxidation of 6-R-5-tetrahydrofolate, which is used as a production raw material to return to the production process of 6-S-5-methyltetrahydrofolate, whil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07D475/04
CPCC07D475/04B01J31/183B01J2531/72B01J2531/847B01J2231/70
Inventor 由君史晓庆喻艳超武文菊朱程
Owner HARBIN UNIV OF SCI & TECH
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