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Method for preparing disodium 5'-ribonucleotide

A technology of nucleotide disodium and nucleoside phosphodiester, which is applied in the fields of food and medicine, can solve the problems of large screening workload and limited scope of substrate action, and achieves reduced post-processing difficulty, fewer impurities and fewer by-products. Effect

Active Publication Date: 2010-11-24
STAR LAKE BIOSCI CO INC ZHAOQING GUANGDONG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that the workload of enzyme screening is very large, and the scope of enzyme substrate action is also limited.

Method used

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  • Method for preparing disodium 5'-ribonucleotide
  • Method for preparing disodium 5'-ribonucleotide
  • Method for preparing disodium 5'-ribonucleotide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Preparation of tert-butoxyphosphoryl dichloride

[0027] Add 30.7g of phosphorus oxychloride and 30ml of dichloromethane into a 100ml reaction flask, cool to below 0°C, add 22.2g of tert-butanol dropwise, then naturally warm up to room temperature and react for 3 hours, first evaporate the solvent under reduced pressure, and then 36.4 g of tert-butoxyphosphoryl dichloride were evaporated under reduced pressure with an oil pump, with a yield of 95.1%.

Embodiment 2

[0029] Synthesis of 5'-guanosine phosphodiester

[0030] Add 40.0 g of tert-butoxyphosphoryl dichloride and 400 ml of dichloromethane into a 1000 ml reaction flask in Example 1, cool to below 0° C., and add 56.6 g of guanosine under nitrogen protection, then add 12 ml of triethylamine, and then Raise the temperature and react at 20-50°C for 5 hours. The reaction was poured into ice water, the organic layer was separated, the aqueous layer was extracted once more with 200ml of dichloromethane, the combined organic layers were washed with water, the organic layer was dried with anhydrous sodium sulfate, filtered, and the solvent was evaporated under reduced pressure. Vacuum-dried to obtain 86.5 g of 5'-guanosine phosphodiester with a yield of 96.8%.

Embodiment 3

[0032] Synthesis of disodium 5'-guanylate

[0033] Add 83.8g of 5'-phosphodiester of guanosine and 1200ml of methanol in Example 2 into a 2000ml reaction flask, pass in an appropriate amount of dry hydrogen chloride gas, then raise the temperature at 20-50°C for 4 hours, and then add sodium hydroxide Solution, neutralization, salt formation, cooling, solid precipitation, filtration, and vacuum drying to obtain 102.6 g of disodium 5'-guanylate with a yield of 96.2% and a purity of 98.3%.

[0034] Above-mentioned embodiment all uses high performance liquid chromatograph purity analysis, and its condition is as follows:

[0035] Instrument: high performance liquid chromatography (Agilent 1200)

[0036] Column: BDS C18 4.6mmx250mm

[0037] Mobile phase: 0.5% potassium dihydrogen phosphate solution

[0038] Flow rate: 1.2ml / sec

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Abstract

The invention provides a method for preparing disodium 5'-ribonucleotide, which comprises the following steps of: preparing phosphoryl dihalide (II), reacting nucleoside with the phosphoryl dihalide (II) to obtain nucleoside phosphodiester (III), and performing R-radical substitution and salifying on the nucleoside phosphodiester (III) to obtain the disodium 5'-ribonucleotide (I). The method has the advantages of high conversion rate, a few byproducts, easy purification, easier impurity removal, reduction in postprocessing difficulty, and capability of preparing the disodium 5'-ribonucleotide with high purity and yield.

Description

technical field [0001] The invention relates to the technical fields of food and medicine, in particular to a new preparation method of 5'-nucleotide disodium. Background technique [0002] Nucleotides have a wide range of uses in the agriculture, food and pharmaceutical industries. Especially in the application of baby food and medicine, it has an irreplaceable function. In the field of medicine, clinical experiments have shown that nucleotides participate in human metabolism, promote the improvement and recovery of internal organs, improve the hematopoietic function of bone marrow, and can be used as an auxiliary drug for the treatment of cancer viruses. It is a very important pharmaceutical raw material. In addition to the application in the pharmaceutical industry, nucleic acid substances also play an important role in the fine chemical and food industries. As one of the ingredients of cosmetics, nucleic acid substances have the functions of skin care and anti-wrinkle....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H1/00C07H1/02C07H19/20C07H19/10
Inventor 任洪发王海波林晓鲁立王晓明欧仁树黄桂基宁异真
Owner STAR LAKE BIOSCI CO INC ZHAOQING GUANGDONG
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