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Preparation method of beta-nicotinamide mononucleotide and purification method

A purification method and single nucleotide technology are applied in the field of preparation of β-nicotinamide mononucleotide, which can solve the problems of many by-products, numerous steps, low yield and the like, and achieve cost savings, improved selectivity, and improved operation. simple effect

Active Publication Date: 2020-06-09
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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  • Preparation method of beta-nicotinamide mononucleotide and purification method
  • Preparation method of beta-nicotinamide mononucleotide and purification method
  • Preparation method of beta-nicotinamide mononucleotide and purification method

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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 , standing for stratification, and collecting the oil 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 furanose substrate ...

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 , standing and stratifying, and collecting the oil 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 substrate intermedia...

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Abstract

The invention discloses a preparation method of beta-nicotinamide mononucleotide and a purification method. The purification method of a furanose substrate intermediate material comprises the following steps: (1) extracting the furanose substrate intermediate material serving as a raw material by adopting a water phase and an oil phase, and collecting a water phase containing a compound shown in aformula I; and (2) extracting the water phase containing the compound shown in the formula I in the step (1) by adopting a phosphorylation auxiliary agent, and collecting a phosphorylation auxiliaryagent phase containing the compound shown in the formula I to obtain a purified furanose substrate intermediate material, wherein the raw material furanose substrate intermediate material is a mixed material containing the compound shown in the formula I, and R1 is one or more of acetyl, bromine, nicotinamide, ethyl nicotinate and butyl nicotinate. The preparation method of the beta-nicotinamide mononucleotide can effectively improve the total yield and purity, the reaction raw materials are cheap and easy to obtain, and the preparation process is simple and 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 Applications(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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