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Preparation method of beta-nicotinamide mononucleotide

A single nucleotide and nicotinamide technology, applied in the field of biomedicine, can solve problems such as product safety hazards, complex processes, and unstable processes

Pending Publication Date: 2020-07-07
EFFEPHARM (SHANGHAI) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention is carried out to solve the above problems, and the purpose is to provide a preparation method of β-nicotinamide mononucleotide, so as to overcome the problems of unstable process, hidden danger of product safety and complicated process in the existing preparation process.

Method used

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  • Preparation method of beta-nicotinamide mononucleotide
  • Preparation method of beta-nicotinamide mononucleotide
  • Preparation method of beta-nicotinamide mononucleotide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Step A: Preparation of Nicotinamide Mononucleotide Sodium Salt:

[0032]

[0033] Nicotinamide ribose chloride (100 g, 0.344 mol) was added into a 2000 mL three-necked flask, and 1000 mL of an aqueous sodium hydroxide solution with pH=9 was added. After the temperature was controlled at 30° C. to stabilize, sodium trimetaphosphate (STMP) (110.48 g, 0.361 mol) was added to react for 4 hours. The reaction process was monitored by high-performance liquid chromatography, and HPLC showed that 85% of the starting material was consumed after 4 hours, and the content of the product nicotinamide mononucleotide accounted for 83%.

[0034] Step B: Preparation of Nicotinamide Mononucleotide

[0035]

[0036] Cool the reaction system to 10°C, add 1M hydrochloric acid, adjust the pH value of the reaction system to 3.5, and acidify the sodium salt of nicotinamide mononucleotide into the internal salt form with structure I.

[0037] Step C: Nicotinamide Mononucleotide Purificat...

Embodiment 2

[0045] Step A: Preparation of Nicotinamide Mononucleotide Potassium Salt:

[0046]

[0047] Nicotinamide ribose chloride (100 g, 0.344 mol) was added into a 2000 mL three-necked flask, and 1000 mL of an aqueous sodium hydroxide solution with pH=9 was added. After the temperature was controlled at 30° C. to stabilize, sodium trimetaphosphate (STMP) (110.48 g, 0.361 mol) was added to react for 4 hours. The reaction process was monitored by high-performance liquid chromatography, and HPLC showed that 79% of the starting material was consumed after 4 hours, and the content of the product nicotinamide mononucleotide accounted for 76%.

[0048] Step B: Preparation of Nicotinamide Mononucleotide

[0049]

[0050] Cool the reaction system to 10°C, add 1ML phosphoric acid, adjust the pH value of the reaction system to 3.5, and acidify the sodium salt of nicotinamide mononucleotide into the internal salt form with structure I.

[0051] Step C: Nicotinamide Mononucleotide Purificat...

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Abstract

The invention relates to the technical field of medicines, and provides a preparation method of beta-nicotinamide mononucleotide. The preparation method comprises the steps of A: performing a phosphorylation reaction: in an aqueous alkaline solution of which the pH is 8-10, and under the condition that the temperature of a reaction system is 25-50 DEG C, enabling nicotinamide riboside and metaphophate to be subjected to the phosphorylation reaction for 2-5h, to obtain an intermediate product of the nicotinamide mononucleotide; B, performing an acidification reaction: adding acid to the reaction solution, regulating the pH value to 3-5, reducing the temperature of the reaction system, and performing acidification on the intermediate product of the beta-nicotinamide mononucleotide to obtainthe beta-nicotinamide mononucleotide; and C, purifying products: sequentially performing filtration with a protein membrane, concentration with a high-pressure desalination membrane, separation and purification with anion exchange resins and concentration and crystallizing on the reaction solution obtained in the step B to obtain pure products of the beta-nicotinamide mononucleotide.

Description

technical field [0001] The invention belongs to the field of biomedicine, and in particular relates to a preparation method of β-nicotinamide mononucleotide. Background technique [0002] NMN (nicotinamide mononucleotide) is an organic molecule and a nucleotide. Many sources of human nutrition contain this substance. It is also the first in the world that has been rigorously scientifically verified to significantly reverse aging and prolong life. revolutionary breakthrough. [0003] The anti-aging effect of nicotinamide mononucleotide was initially discovered by the David Sinclair laboratory of Harvard University in 2014, and from 2016 to 2018, the world's top scientific research institutions such as Harvard Medical School, Washington University, Japan's Kei University, etc. , inhibiting cognitive decline caused by aging, reversing vascular death, and protecting cardiovascular and cerebrovascular functions have proved its remarkable effect of inhibiting aging and prolonging...

Claims

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Application Information

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IPC IPC(8): C07H1/00C07H1/06C07H19/048
CPCC07H1/00C07H1/06C07H19/048
Inventor 徐钦源余建军胡健
Owner EFFEPHARM (SHANGHAI) CO LTD
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