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Low-energy-consumption preparation method for synthesizing high-purity folic acid

A high-purity, low-energy-consumption technology, applied in the direction of organic chemistry, can solve the problem of low folic acid purity, achieve the effects of shortening reaction time, saving costs, and reducing energy consumption

Active Publication Date: 2016-03-30
北京斯利安药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently available folic acid in the market is relatively low in purity, mostly containing impurity A (N-p-aminobenzoyl glutamic acid), impurity D (pteroic acid), and other impurities are also relatively high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 350L of water into the 500L reaction kettle, stir, and the temperature of the system is raised to 45°C. Add 2.1 kg of sodium acetate, 7.0 kg of sodium metabisulfite, 3.0 kg of 2,4,5 triamino-6-hydroxypyrimidine sulfate, and 3.5 kg of N-p-aminobenzoyl glutamic acid in one batch. Slowly add 4.5 kg of trichloroacetone, react for 4 hours after the dropwise addition, and adjust the pH to 3.3 with 40% sodium hydroxide aqueous solution at the time of reaction for 0.5 hours. After the reaction was completed, the temperature was lowered to normal temperature, and the pH was adjusted to 3.3 with 40% aqueous sodium hydroxide solution. Shake off and filter to obtain folic acid crude product. Beat the crude product with 40L of 7% hydrochloric acid solution at room temperature for 0.5h, filter through a filter cloth, add 0.3kg of magnesium oxide into 25L of water at 80°C, then add the acid-washed filter cake, stir for 0.5 hour, add 0.1kg of activated carbon, 80 °C stirring was ...

Embodiment 2

[0026] Add 350L of water into the 500L reaction kettle, stir, and the temperature of the system is raised to 40°C. Add 2.5 kg of sodium acetate, 6.0 kg of sodium metabisulfite, 3.0 kg of 2,4,5 triamino-6-hydroxypyrimidine sulfate, and 4.5 kg of N-p-aminobenzoyl glutamic acid in one batch. Slowly add 5.5 kg of trichloroacetone, react for 5 hours after the dropwise addition, and adjust the pH to 3.3 with 40% sodium hydroxide aqueous solution during the reaction for 1 hour. After the reaction, the temperature was lowered to normal temperature, and the pH was adjusted to 3.3 with 40% aqueous sodium hydroxide solution. Shake off and filter to obtain folic acid crude product. Beat the crude product with 40L of 10% hydrochloric acid solution at room temperature for 1 hour, filter through a filter cloth, add 0.9kg of magnesium oxide to 25L of water at 80°C, then add acid-washed filter cake, stir for 1 hour, add 0.2kg of activated carbon, Stirring was continued for 1 hour. Filter wh...

Embodiment 3

[0028] Add 350L of water into the 500L reaction kettle, stir, and the temperature of the system is raised to 50°C. Add 1.5 kg of sodium acetate, 8.0 kg of sodium metabisulfite, 3.0 kg of 2,4,5 triamino-6-hydroxypyrimidine sulfate, and 4.0 kg of N-p-aminobenzoyl glutamic acid in one batch. Slowly add 3.5 kg of trichloroacetone, react for 3 hours after the dropwise addition, and adjust the pH to 3.3 with 40% sodium hydroxide aqueous solution at the time of reaction for 0.5 hours. After the reaction was completed, the temperature was lowered to normal temperature, and the pH was adjusted to 3.3 with 40% aqueous sodium hydroxide solution. Shake off and filter to obtain folic acid crude product. Beat the crude product with 40L of 14% hydrochloric acid solution at room temperature for 0.75h, filter through a filter cloth, add 0.6kg of magnesium oxide into 25L of water at 80°C, then add acid-washed filter cake, stir for 0.75h, add 0.15kg of activated carbon, 80 °C stirring was cont...

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Abstract

The invention discloses a low-energy-consumption preparation method for synthesizing high-purity folic acid. The method comprises adding 2,4,5-triamino-6-hydroxypyrimidine sulfate, p-aminobenzamide glutamic acid, trichloroacetone, sodium acetate and sodium pyrosulfite into water, performing docking reaction, adjusting pH by adding solid sodium acetate before the reaction is started and separately adding a sodium hydroxide solution during reaction and after the reaction is finished, and filtering; performing acid-washing and filtering in hydrochloric acid solution; adding a magnesium oxide solution into water for reaction, adding active carbon for decoloring, and filtering; adjusting pH value by using hydrochloric acid, cooling and filtering; and washing with purified water and filtering, drying the filter cake, so as to obtain the final product. By using the method for producing folic acid, energy consumption is reduced, also yield and product purity are improved, and also cost is substantially saved.

Description

technical field [0001] The invention relates to the field of pharmaceutical preparations, in particular to a preparation method for synthesizing high-purity folic acid with low energy consumption. Background technique [0002] As a basic vitamin, folic acid is named for its rich content in plant green leaves. Most of the folic acid currently on the market is prepared by chemical synthesis. Its traditional synthesis method is to use N-p-aminobenzoyl glutamic acid, 2,4,5-triamino-6-hydroxypyrimidine sulfate and trichloroacetone to dock to prepare crude folic acid, and then refine it by acid dissolution and alkali To prepare pure folic acid, the folic acid production method without sewage discharge mentioned in the patent CN101323614B has a crude product yield of 85% and a refined process yield of 60%. The folic acid currently available on the market is relatively low in purity, mostly containing impurity A (N-p-aminobenzoyl glutamic acid), impurity D (pteroic acid), and other...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D475/04
Inventor 易斌安明榜韩妮娜
Owner 北京斯利安药业有限公司
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