Preparation method of tetrahydrofolic acid

A technology of tetrahydrofolate and dihydrofolate, applied in the direction of organic chemistry and the like, can solve the problems of incomplete reduction reaction, large loss, low yield, difficult separation, etc., and achieves no by-product generation, low raw material consumption, and short process route. Effect

Inactive Publication Date: 2011-01-19
湖北省琴断口监狱
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above two methods all use high-purity folic acid as a synthetic raw material. In industry, folic acid with medicinal specifications is made into magnesium salt, and then refined, resulting in large losses and low yield. The refined yield of folic acid is generally below 60%, and the process is complicated. ,high cost
Not only that, the biggest shortcoming of the above two methods is that the reduction reaction is not complete under mild synthesis conditions, resulting in a large amount of dihydrofolate
When the synthesis conditions are severe, the molecule breaks to produce pterin and p-aminobenzoyl glutamic acid (PADGA), which reduces the yield and makes separation difficult

Method used

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  • Preparation method of tetrahydrofolic acid
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] A preparation method of tetrahydrofolate, the steps are as follows:

[0017] 1. Dissolve 10g of sodium dithionite (sodium dithionite) in 150ml of pure water, and use a 250ml Erlenmeyer flask as the reaction vessel;

[0018] 2. Put 10g of folic acid into 1, add 2.4g of sodium hydroxide to dissolve the folic acid, at this time the pH is 9.0, and the solution is brownish red;

[0019] 3. Seal the mouth of the bottle with plastic wrap, pierce 2 pinholes to exhaust air, and synthesize for 3 hours; control the synthesis temperature at 15-20°C;

[0020] 4. Put 7g of potassium borohydride into 3, seal the mouth of the bottle with plastic wrap, pierce 2 pinholes to exhaust air, and synthesize at 15-20°C for 3 hours; the synthetic liquid is light brown, pH 10.50;

[0021] 5. Use 3M hydrochloric acid to adjust the pH of the synthetic solution to 3.5; filter under nitrogen to obtain off-white crystals, and the mother liquor is colorless;

[0022] 6. The wet product was washed thr...

Embodiment 2

[0024] A preparation method of tetrahydrofolate, the steps are as follows:

[0025] 1. Add 1200ml of pure water to a 3000ml beaker, add 24g of sodium hydroxide and 96g of dithionous acid under stirring, and stir to dissolve them completely;

[0026] 2. Weigh 120g of folic acid, add it to 1, stir to dissolve it completely, transfer it to a 3L glass synthesis kettle, start the synthesis kettle to stir, the rotation speed is 150rmp, the temperature is 25°C; the synthesis is 4 hours, and the pH is 5.50 at this time;

[0027] 3. Weigh 60g of potassium borohydride, add it to 2 in batches, and react at 20-25°C for 120 minutes, the synthetic liquid is light brown, pH 7.5;

[0028] 4. Mix the liquid with 3M hydrochloric acid at pH 3.0, filter it under the protection of nitrogen to obtain off-white crystals, and the mother liquor is colorless;

[0029] 5. Stir and wash the crystals with 1500ml of deionized oxygen-free ice water for 3 times, and filter under nitrogen protection to obtai...

Embodiment 3

[0032] A preparation method of tetrahydrofolate, the steps are as follows:

[0033] 1. Add 300L of pure water to a 500L stainless steel synthesis kettle, add 6kg of sodium hydroxide and 24kg of dithionous acid under stirring, and stir to dissolve them completely;

[0034] 2. Add 30kg of folic acid into the kettle, stir to completely dissolve, control the reaction temperature at 25-30°C, synthesize for 5 hours, and the pH at this time is 5.5;

[0035] 3. Add 18kg of potassium borohydride to 2 in batches, and react at 25-30°C for 2 hours, the synthetic liquid is light brown, pH 8.5;

[0036] 4. Mix the liquid with 3M hydrochloric acid at pH 3.0, filter it under the protection of nitrogen to obtain off-white crystals, and the mother liquor is colorless;

[0037] 5. Stir and wash the wet product with 300L deionized oxygen-free ice water to wash the crystals, and filter under the protection of nitrogen to obtain off-white crystals;

[0038] 6. Place the wet product in a vacuum fr...

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Abstract

A preparation method of tetrahydrofolic acid comprises steps of adopting industrial folic acid as raw material and adopting sodium hydrosulfite and potassium borohydride synergic reduction method to synthesize tetrahydrofolic acid under mild condition. The method has the advantages of short and simple processes, mild condition, easy operation, no noble metals such as platinum dioxide and the like, low raw material consumption, no by-product and high yield.

Description

Technical field [0001] The present invention involves the field of biochemical and pharmaceutical technology. Specifically, it is a method of preparation of tetrahydrinic acid. Background technique [0002] Tethel acid is an intermediate for synthetic antitumor drugs 5-calcium-ampotate.In recent years, 5-metharhydroccalone is also widely used in the treatment of giant nucleus red blood cell anemia, psoriasis and rheumatoid arthritis.At the same time, tetrahydrogen folic acid is an important raw material for the production of L-serine to produce L-seritic acid by using mrythic hydroxytic metastase enzymes.It is involved in the metabolism of serumine, glycine, histidine, and sprinine in the body.It is the carbon unit's carrier and coenzyme.Widely used in biology, chemical industry, pharmaceutical, biochemical research and other fields.Has a very important biological role. [0003] Because 5-calcium-hydrogen folic acid is widely used in the clinic and tetrahydrofolate is widely used...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D475/04
Inventor 徐新平
Owner 湖北省琴断口监狱
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