Preparation method of uridine-5'-monophosphate disodium

A technology of disodium uridine and cytidylic acid, which is applied to the preparation of sugar derivatives, chemical instruments and methods, and sugar derivatives, and can solve problems such as strong polarity, increased workload, and time-consuming

Active Publication Date: 2015-03-25
美亚药业海安有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The phosphorylated product has many impurities and the direct product 5'-uridine acid has strong polarity, which leads to difficult purification, time-consuming, low yield and high production cost
The deamination method is to use cytidylic acid as a raw material, and through a one-step deamination reaction, cytidylic acid is directly converted into uridine acid. However, in the prior art, it is necessary to go through at least three processes to obtain the crude product of 5'-uridine disodium. Steps: synthetic reaction→steam distillation→vacuum distillation, and the last two steps require special equipment, which increases energy consumption and increases workload

Method used

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  • Preparation method of uridine-5'-monophosphate disodium
  • Preparation method of uridine-5'-monophosphate disodium
  • Preparation method of uridine-5'-monophosphate disodium

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preparation example Construction

[0029] The invention provides a kind of preparation method of 5'-uridine acid disodium, described method is made up of following steps:

[0030] In the first step, mix cytidylic acid (CMP) or its sodium salt, sodium nitrite and water, add acid and / or acid anhydride dropwise within 60°C, and continue to react for 0-6 hours after the dropwise addition to obtain the reaction Solution 1;

[0031] In the second step, when the residual amount of CMP is lower than 1%, adjust the pH value of the reaction solution 1 to 6.4-7.2 to obtain the reaction solution 2;

[0032] The third step is to mix the reaction solution 2 with 0.5-10 times the amount of 95v / v% ethanol (that is, the volume of 95% ethanol: the volume of the reaction solution 2 = 0.5-10, which is the volume ratio V / V), crystallize and filter to obtain Crude disodium 5'-uridine acid;

[0033] The fourth step is to mix the crude product of 5'-uridine disodium with water, adjust the pH value to 7.0-8.5, and obtain the reaction...

Embodiment 1

[0063] In the dry 1000m1 four-necked bottle, install an exhaust gas absorption device, a mechanical stirring device, and a material dropping device. Add 50g cytidylic acid, 150ml deionized water, stir to dissolve. Add 50g of sodium nitrite and stir to dissolve. Start to add hydrochloric acid dropwise, and add 50ml of hydrochloric acid in total. After the dropwise addition of hydrochloric acid, continue the reaction for 2 hours, and control the temperature below 50°C during the whole process. Sampling was detected by HPLC method, and the residual amount of CMP was 0.27%. Use liquid caustic soda to adjust the pH value of the reaction solution to 6.4-7.2, add 2 times the amount of 95% ethanol to crystallize, and filter to obtain the crude product of disodium 5'-uridine acid. Add an appropriate amount of water to the above crude product to dissolve, adjust the pH value of the reaction solution to 7.0-8.5 with liquid caustic soda, recrystallize with twice the amount of ethanol, f...

Embodiment 2

[0068] In the dry 1000m1 four-necked bottle, install an exhaust gas absorption device, a mechanical stirring device, and a material dropping device. Add 50g cytidylic acid, 150ml deionized water, stir to dissolve. Add 100g of sodium nitrite and stir to dissolve. Start to add acetic acid dropwise, add 50ml of acetic acid in total, after the acetic acid has been added dropwise, continue to react for 3 hours, and control the temperature in the whole process below 50°C. Sampling was detected by HPLC method, and the residual amount of CMP was 0.15%. Use liquid caustic soda to adjust the pH value of the reaction solution to 6.4-7.2, add 2 times the amount of 95% ethanol to crystallize, and filter to obtain the crude product of disodium 5'-uridine acid. Add an appropriate amount of water to the above crude product to dissolve, adjust the pH value of the reaction solution to 7.0-8.5 with liquid caustic soda, recrystallize with 3 times the amount of ethanol, filter and dry to obtain ...

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Abstract

The invention discloses a preparation method of uridine-5'-monophosphate disodium. The method comprises the following steps: (1) mixing cytidine monophosphate (CMP) or sodium salt, sodium nitrite and deionized water, dropwise adding acid and / or acid anhydride, continuously reacting for 0-6 hours after completing dropwise adding to obtain reaction solution 1; (2) if residual quantity of CMP is lower than 1%, adjusting the pH value of the reaction solution 1 to 6.4-7.2 to obtain reaction solution 2; (3) mixing the reaction solution 2 and 95v / v% of ethyl alcohol, crystallizing and filtering to obtain a uridine-5'-monophosphate disodium crude product; (4) mixing the uridine-5'-monophosphate disodium crude product and water, and adjusting the pH value to 7.0-8.5 to obtain reaction solution 3; and (5) mixing the reaction solution 3 and an organic solvent, recrystalizing and filtering to obtain the uridine-5'-monophosphate disodium.

Description

technical field [0001] The invention relates to the field of nucleotide preparation, in particular to a preparation method of disodium 5'-uridine acid. Background technique [0002] Disodium 5'-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 diphosphate glucose, 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 stepped up research and development efforts on disodium 5'-uridine acid. [0004] At present, the methods for preparing disodium 5'-uridine ...

Claims

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Application Information

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IPC IPC(8): C07H19/10C07H1/00
CPCC07H1/00C07H19/10
Inventor 王宏傅得响卢凰姗
Owner 美亚药业海安有限公司
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