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Production technology for riboflavin sodium phosphate

A technology of riboflavin sodium phosphate and production process is applied in the field of chemical preparation technology of riboflavin sodium phosphate, which can solve the problems of low content of riboflavin sodium phosphate, large amount of polluted waste liquid treatment, low quality, etc. The effect of low content, simple process and stable quality

Inactive Publication Date: 2017-10-24
山西集翔生物工程有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The product produced by the above synthesis method has a low content of riboflavin sodium phosphate, which is difficult to meet the requirements of "Chinese Pharmacopoeia", and the content of related substances riboflavin diphosphate and free phosphoric acid are relatively high; there are many impurities and the quality is not high ; Large amount of polluted waste liquid treatment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1. Phosphorylation reaction

[0026] ⑴Put 42.55g of phosphorus oxychloride and 59g of acetonitrile into the reaction vessel in turn, lower the temperature to 10°C, first drop 14.67g of pyridine into the reaction solution, and then slowly add the pyridine solution (7.3g of pyridine→3mL of purified water), and the reaction For 30 minutes, the temperature was controlled not to exceed 25°C; 25g of vitamin B2 was added to carry out the phosphorylation reaction. The reaction temperature is controlled at 35°C, the stirring speed is controlled at 60rpm-80rpm, and the reaction time is 30 minutes;

[0027] (2) Add 100 mg of riboflavin cyclic phosphate seed crystals, stir and crystallize for 60 minutes; separate riboflavin cyclic phosphate crystals.

[0028] 2. Hydrolysis reaction

[0029] Prepare 43.2ml of 18% hydrochloric acid solution, add riboflavin cyclic phosphate crystals to carry out hydrolysis reaction. The reaction temperature is controlled at 50°C, the stirring speed...

Embodiment 2

[0042] 1. Phosphorylation reaction

[0043] ⑴Put 42.55g of phosphorus oxychloride and 59g of acetonitrile into the reaction vessel in turn, cool down to 10°C, first drop 14.67g of pyridine into the reaction solution, and then slowly add the pyridine solution (7.3g of pyridine→2.9mL of purified water), React for 30 minutes, and control the temperature not to exceed 25°C; add 25g of vitamin B2 to carry out the phosphorylation reaction. The reaction temperature is controlled at 35°C, the stirring speed is controlled at 60rpm-80rpm, and the reaction time is 20 minutes;

[0044] (2) Add 50 mg of riboflavin cyclic phosphate seed crystals, stir and crystallize for 40 minutes; separate riboflavin cyclic phosphate crystals.

[0045] 2. Hydrolysis reaction

[0046] Prepare 46ml of 18% hydrochloric acid solution, add riboflavin cyclic phosphate crystals to carry out hydrolysis reaction. The reaction temperature is controlled at 55°C, the stirring speed is controlled at 80rpm-100rpm, a...

Embodiment 3

[0059] 1. Phosphorylation reaction

[0060] ⑴Put 50.62g of phosphorus oxychloride and 71.51g of acetonitrile into the reaction vessel in turn, cool down to 10°C, first drop 16g of pyridine into the reaction solution, then slowly add the pyridine solution (8g of pyridine→3.2mL of purified water), and react For 45 minutes, the temperature was controlled not to exceed 25°C; 25g of vitamin B2 was added to carry out the phosphorylation reaction. The reaction temperature is controlled at 35°C, the stirring speed is controlled at 60rpm-80rpm, and the reaction time is 30 minutes;

[0061] (2) Add 100 mg of riboflavin cyclic phosphate seed crystals, stir and crystallize for 60 minutes; separate riboflavin cyclic phosphate crystals.

[0062] 2. Hydrolysis reaction

[0063] Prepare 50ml of 18% hydrochloric acid solution, add riboflavin cyclic phosphate crystals to carry out hydrolysis reaction. The reaction temperature is controlled at 45°C, the stirring speed is controlled at 80rpm-1...

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Abstract

The invention relates to a production technology for riboflavin sodium phosphate. The invention aims to realize simple technology, easy control and high yield. The production technology comprises the following steps: performing phosphorylation reaction: adding phosphorus oxychloride and acetonitrile in turn, dropwise adding pyridine of which the weight is 2 / 3 of the total weight, slowly dropwise adding a solution prepared from the residual pyridine and purified water and reacting for 30-60 minutes; adding vitamin B2 for performing phosphorylation reaction for 20-40 minutes under the temperature at 30-37 DEG C; while crystallizing, adding riboflavin cyclophosphate seed crystal of which the weight is 0.25-0.5% of the weight of the vitamin B2 for promoting the crystallization; performing hydrolysis reaction: adding 18%-20% hydrochloric acid solution into the separated riboflavin cyclophosphate crystal and performing hydrolysis reaction for 1-3 hours under the temperature at 45-55 DEG C; adding sodium hydroxide for performing neutral reaction and separating, thereby acquiring a riboflavin sodium phosphate crude product; washing with methyl alcohol and ethanol solution and removing the impurities and organic residual matters from the riboflavin sodium phosphate; drying and crushing to the required particle size.

Description

technical field [0001] The invention relates to a chemical preparation process of riboflavin sodium phosphate, which belongs to the technical field of medicinal chemistry. Background technique [0002] Riboflavin sodium phosphate is a derivative product of vitamin B2. Because of its excellent water solubility, it can be made into injection solution for subcutaneous, intramuscular or intravenous injection. The problem that vitamin B2 can only be taken orally and cannot be made into injections is solved. Its role is the same as that of vitamin B2, and it is a part of the prosthetic group of diaphorase in the body. Yellow enzyme plays a hydrogen transfer role in biological redox and has the following physiological functions: 1. It can participate in the metabolism of carbohydrates, proteins, nucleic acids and fats. Improve the body's utilization of protein and promote growth and development. 2. Participate in the growth and metabolism of cells, and is an essential nutrient fo...

Claims

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Application Information

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IPC IPC(8): C07F9/6561
CPCC07F9/65618C07B2200/13
Inventor 齐延红付春生张龙霞杨宇鹏韩进功左小舟潘夏萌
Owner 山西集翔生物工程有限公司
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