New method for synthesizing uridylic acid disodium

A technology of disodium uridine acid and a new method, which is applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., can solve the problems of high production cost, difficult purification, low yield, etc., and achieve low production cost , stable process and high product purity

Active Publication Date: 2011-11-23
宋道淮
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the strong polarity of the direct product of the chemical synthesis method, 5'-uridine acid, it is difficult to purify, time-consuming, low in yield, and high in production cost.

Method used

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  • New method for synthesizing uridylic acid disodium
  • New method for synthesizing uridylic acid disodium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] In a dry 500ml four-necked bottle, install a reflux condenser and a mechanical stirring device. Add 20 grams of 5′-cytidylic acid and 100 ml of deionized water, stir to dissolve. Add 4.31 g of sodium nitrite and stir to dissolve. Use an ice-salt bath to lower the temperature of the inner liquid to -5°C, start adding sulfuric acid dropwise, and strictly control the temperature during the entire dropping process at -5°C to 0°C. A total of 40 grams of sulfuric acid is added.

[0019] After adding sulfuric acid, remove the ice-salt bath. The temperature of the above solution was slowly raised to 60° C. within 30 minutes, and after stirring for 1 hour, the reaction liquid was detected by HPLC until there was no 5′-cytidylic acid raw material, and the reaction was terminated. Subsequently, water vapor is directly introduced into the reaction flask to carry out steam distillation. Stop distillation when there are no more oil droplets in the distillate.

[0020] The collect...

Embodiment 2

[0023] In a dry 500ml four-necked bottle, install a reflux condenser and a mechanical stirring device. Add 20 grams of 5′-cytidylic acid and 300 ml of deionized water, stir to dissolve. Add 21.40 g of sodium nitrite and stir to dissolve. The temperature of the inner liquid was lowered to -5°C with an ice-salt bath, and sulfuric acid was added dropwise. During the entire dropping process, the temperature was strictly controlled at -5°C to 0°C. A total of 320 grams of sulfuric acid was added.

[0024] After adding sulfuric acid, remove the ice-salt bath. The temperature of the above solution was slowly raised to 10° C. within 30 minutes, and after stirring for 20 hours, the reaction solution was detected by HPLC to have no 5′-cytidine raw material, and the reaction was terminated. Subsequently, water vapor is directly introduced into the reaction flask to carry out steam distillation. Stop distillation when there are no more oil droplets in the distillate.

[0025] The colle...

Embodiment 3

[0028] In a dry 500ml four-necked bottle, install a reflux condenser and a mechanical stirring device. Add 20 grams of 5′-cytidylic acid and 180 ml of deionized water, stir to dissolve. Add 6.47 g of sodium nitrite and stir to dissolve. Use an ice-salt bath to lower the temperature of the inner liquid to -5°C, start adding acetic acid dropwise, and strictly control the temperature during the entire dropping process at -5°C to 0°C. Add 60 grams of acetic acid in total.

[0029] After adding acetic acid, remove the ice-salt bath. The temperature of the above solution was slowly raised to 50° C. within 30 minutes, and after stirring for 3 hours, the reaction solution was detected by HPLC to have no 5′-cytidylic acid raw material, and the reaction was terminated. Subsequently, water vapor is directly introduced into the reaction flask to carry out steam distillation. Stop distillation when there are no more oil droplets in the distillate.

[0030] The collected aqueous solutio...

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Abstract

The invention discloses a new method for synthesizing uridylic acid disodium. The method comprises the following steps: adding cytidylic acid and sodium nitrite in deionized water, and dropwise adding inorganic or organic acid at the constant temperature of minus 5 DEG C-0 DEG C; stirring the solution and heating to 10-60 DGE C, reacting for 1-12 hours, and introducing steam for steam distillation after the reaction is finished so as to obtain a uridylic acid solution; regulating the pH of the uridylic acid solution to 7.0-8.5 with alkali, distilling at reduced pressure until a liquid is not distilled out; adding 95% ethanol the weight of which is 3-12 times that of cytidylic acid, heating and refluxing for 0.5-6 hours under the condition of stirring, crystallizing, and filtering so as to obtain crude uridylic acid disodium; and dissolving crude uridylic acid disodium in a proper amount of water, recrystallizing with ethanol the weight of which is 1-3.5 times that of the crude uridylic acid disodium, filtering and drying so as to obtain the uridylic acid disodium product. By using the method, the yield of uridylic acid disodium is above 92.75%, the purity of uridylic acid disodium by detection of high performance liquid chromatography (HPLC) is more than 99.50%, and the purity of uridylic acid disodium by detection of ultraviolet (UV) light is above 98.50%. The method has the advantages of simple and reasonable process, good product quality stability, low production cost and the like, and is easy to be applied to massively production.

Description

technical field [0001] The invention relates to a preparation method of disodium uridine acid Background technique [0002] Disodium uridine can be used as an important intermediate in the production of nucleic acid drugs, health food and biochemical reagents. It is also used in the manufacture of uridine triphosphate, polyadenylic acid and other drugs, and plays an important role in the treatment of many major diseases. [0003] At present, with the expansion of the application range of uridine triphosphate, diuridine tetraphosphate, and uridine phosphatase inhibitors in the field of medicine, and the application of uridine diphosphate glucose pyrophosphorylase gene, domestic and foreign scientific research institutions and Enterprises have also increased the research and development of disodium uridine acid. At present, the methods for preparing disodium uridine mainly include enzymatic hydrolysis and chemical synthesis. [0004] Enzymatic hydrolysis to produce disodium...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H19/10C07H1/00
Inventor 宋道淮宋同和
Owner 宋道淮
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