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A preparation method and purification method of β-nicotinamide mononucleotide

A purification method and nicotinamide technology are applied in the preparation of sugar derivatives, chemical instruments and methods, organic chemistry, etc., and can solve the problems of many by-products, many steps, low yield, etc., and achieve improved selectivity, simple operation, cost saving effect

Active Publication Date: 2021-09-21
SHANGHAI CHANGFA NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is to provide a kind of β-nicotinamide in order to overcome the defects of many steps, many by-products, low yield and difficult purification in the method of chemically synthesizing β-nicotinamide mononucleotide in the prior art. Preparation method and purification method of mononucleotide

Method used

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  • A preparation method and purification method of β-nicotinamide mononucleotide
  • A preparation method and purification method of β-nicotinamide mononucleotide
  • A preparation method and purification method of β-nicotinamide mononucleotide

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preparation example Construction

[0046] The preparation method of the raw material furanose substrate intermediate material comprises the following steps:

[0047] Step (1) Add 800 mL of dichloromethane and 80 g of tetraacetyl ribose into a 2L glass reactor, and start stirring. Turn on the circulating water in the jacket, and when the internal temperature reaches 12°C, add 5.6 g of trimethylsilyl trifluoromethanesulfonate with a constant pressure dropping funnel, and drop it in 20 minutes. 6g of nicotinyl ethyl ester was added, the temperature of the circulating water was raised, and when the temperature reached 49° C., the reaction was kept for 4 hours. After using HPLC to monitor that the remaining ethyl nicotinate was less than 5%, the solvent was evaporated to dryness under a vacuum of -0.09MPa.

[0048] Step (2) Pour 1L of methanol pre-cooled to 10°C into the system, start stirring to dissolve the material, turn on the circulating water of the reactor, and after the internal temperature reaches -5°C, pass...

Embodiment 1

[0051] Step 1: adopt the preparation method of the above-mentioned raw material furanose substrate intermediate material to obtain the raw material furanose substrate intermediate material; in the step (2) of the preparation method of the raw material furanose substrate intermediate material, the solvent removal process is carried out in a rotary evaporator Carry out solvent removal treatment at a vacuum of -0.09MPa and a temperature of 10°C, and recover the solvent.

[0052] Step 2: Transfer the furanose substrate intermediate material into a 2L flask, pour into 380g of water and 220g of dichloromethane, mix under stirring conditions, the mixing time is 12min, and transfer to a 2L separatory funnel after mixing In the method, stand and separate layers, and collect the aqueous phase containing the compound shown in formula I; the mass ratio of water to the raw material furanose substrate intermediate material is 8:1; the mass ratio of dichloromethane to the raw material furanos...

Embodiment 2

[0056] Step 1: adopt the preparation method of the above-mentioned raw material furanose substrate intermediate material to obtain the raw material furanose substrate intermediate material; in the step (2) of the preparation method of the raw material furanose substrate intermediate material, the solvent removal process is carried out in a rotary evaporator Carry out solvent removal treatment at a vacuum of -0.085MPa and a temperature of 15°C, and recover the solvent.

[0057] Step 2: Transfer the raw furanose substrate intermediate material into a 1L flask, pour into 140g of water and 100g of ethyl acetate, mix under stirring, the mixing time is 10min, and transfer to a 1L separatory funnel after mixing In the method, stand for stratification, and collect the aqueous phase containing the compound shown in formula I; the mass ratio of water to the raw material furanose substrate intermediate material is 10:1; the mass ratio of dichloromethane to the raw material furanose substr...

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Abstract

The invention discloses a preparation method and purification method of β-nicotinamide mononucleotide. The method for purifying the furanose substrate intermediate material comprises the following steps: (1) extracting the raw material furanose substrate intermediate material with water phase and oil phase, and collecting the water phase containing the compound shown in formula I; (2) using phosphorylation The auxiliary agent extracts the aqueous phase containing the compound shown in formula I in step (1), collects the phosphorylation auxiliary phase containing the compound shown in formula I, and obtains the purified furanose substrate intermediate material; wherein, the raw material furanose substrate The intermediate material of the product is a mixed material comprising a compound represented by formula I, wherein R1 is one or more of acetyl, bromo, nicotinamide, ethyl nicotinate and butyl nicotinate. The preparation method of β-nicotinamide mononucleotide in the present invention can effectively improve the total yield and purity, the reaction raw materials are cheap and easy to obtain, the preparation process is simple, and it is suitable for industrial production.

Description

technical field [0001] The invention specifically relates to a preparation method and purification method of β-nicotinamide mononucleotide. Background technique [0002] β-nicotinamide mononucleotide is a naturally occurring bioactive nucleotide, which can be synthesized in the human body and can also be ingested from daily vegetables and meat. It is closely related to human immunity and metabolism. [0003] [0004] The function of β-nicotinamide mononucleotide in the body is mainly reflected by nicotinamide adenine dinucleotide, which is widely distributed in all cells and participates in thousands of biocatalytic reactions. In recent years, the anti-aging effect of nicotinamide adenine dinucleotide has attracted widespread attention in the scientific community. A large number of animal experiments have shown that after increasing the content of nicotinamide adenine dinucleotide, the aging organs can be restored to their youthful state, while supplementing β-nicotinami...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H1/02C07H1/00C07H1/06C07H19/048C07D307/20
CPCC07D307/20C07H1/00C07H1/02C07H1/06C07H19/048
Inventor 施晓旦潘航郑小群
Owner SHANGHAI CHANGFA NEW MATERIAL CO LTD
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