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Synthesis method and synthesis device of beta-nicotinamide mononucleotide

A single nucleotide and synthetic method technology, applied in the chemical field, can solve the problems of low reaction yield, unstable process, difficult purification of reaction intermediates and products, etc., and achieve the effect of reducing production costs and safe and reliable operation

Inactive Publication Date: 2020-11-17
青岛新通道合成技术有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The current production method of β-nicotinamide mononucleotide is mainly to use nicotinamide and ribose as raw materials through condensation, deacetylation, and phosphorylation (see Chem.Commun.1999, 729-730), but there are reactions Low efficiency, difficulty in purification of reaction intermediates and products, unstable process and difficulty in scaling up, etc.

Method used

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  • Synthesis method and synthesis device of beta-nicotinamide mononucleotide
  • Synthesis method and synthesis device of beta-nicotinamide mononucleotide
  • Synthesis method and synthesis device of beta-nicotinamide mononucleotide

Examples

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no. 1 example

[0026] Please refer to figure 1 , the synthetic method of β-nicotinamide mononucleotide comprises the following steps:

[0027] S1 condensation reaction, add 70 grams of ethyl nicotinate, 100 grams of tetraacetyl ribose and 1000 grams of chloroform into the reaction kettle, stir and dissolve at room temperature, then add 10 grams of trimethylsilyl trifluoromethanesulfonate in chloroform 100 grams of the solution, and then carry out condensation reaction at 50°C for 1 hour. After the reaction, cool down to room temperature, add 20 grams of ethanol to quench the reaction, remove the solvent under reduced pressure, and obtain 150 grams of triacetyl nucleoside containing nicotinic acid ethyl ester;

[0028] S2: Deacetylation, dissolve 150 grams of nicotinic acid ethyl triacetyl nucleoside in S1 in 1500 grams of ethanol, add dropwise an ethanol solution of 30 grams of sodium ethoxide at 0°C, react for 2 hours, and dropwise add Hydrochloric acid to neutrality, then add methyl tert-...

no. 2 example

[0037] Please refer to figure 2 , a synthesis device for β-nicotinamide mononucleotide, which is applied to the synthesis method of β-nicotinamide mononucleotide, comprising: two mixing tanks 1, a first section tube reactor 3, purified water Tank 5, ammonia gas tank 7, second stage pipe reactor 8 and discharge tank 10; first metering pump 2, said first metering pump 2 is fixedly installed on said mixing tank 1, and said first metering The pump 2 is in communication with the mixing tank 1; the first reaction tube 4, the first reaction tube 4 is fixedly installed in the first section tube reactor 3, and the first reaction tube 4 is connected with the first metering The pump 2 is communicated with the ammonia gas tank 7; the second metering pump 6, the second metering pump 6 is fixedly installed on the pure water tank 5, and the second metering pump 6 is connected to the pure water tank 5 and The first reaction tube 4 communicates; the second reaction tube 9, the second reactio...

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Abstract

The invention provides a synthesis method of beta-nicotinamide mononucleotide. The synthesis method of the beta-nicotinamide mononucleotide comprises the following steps: S1, condensation reaction: adding ethyl nicotinate, tetraacetylribose and a solvent A into a reaction kettle, performing stirring and dissolving at room temperature, dropwise adding a solution of a catalyst A, carrying out condensation reaction at 50 DEG C for 1 hour, cooling to room temperature after the reaction is finished, adding ethanol for quenching reaction, and removing the solvent under reduced pressure, and obtaining triacetyl nucleoside containing ethyl nicotinate; and S2, deacetylation: dissolving the ethyl nicotinate triacetyl nucleoside obtained in the step S1 into ethanol, and dropwise adding organic alkaliat 0 DEG C. The synthesis method of beta-nicotinamide mononucleotide provided by the invention has the advantages that two steps of phosphorylation and ammonolysis are integrated into one step, leakage of dangerous materials such as phosphorus oxychloride and ammonia gas and the like is avoided, the operation is safe and reliable, and the production cost is greatly reduced.

Description

technical field [0001] The invention relates to the technical field of chemistry, in particular to a synthesis method and a synthesis device of β-nicotinamide mononucleotide. Background technique [0002] β-nicotinamide mononucleotide is a health product that has received extensive research and attention in recent years, and it is also a key intermediate for the synthesis of nicotinamide adenine dinucleotide (coenzyme I). It is reported that β-nicotinamide mononucleotide plays an important role in immune system regulation, energy metabolism regulation and insulin secretion regulation, etc. It has great potential in anti-aging, diabetes treatment and other aspects, and has related health care in Japan and the United States The product goes on sale. [0003] The current production method of β-nicotinamide mononucleotide is mainly to use nicotinamide and ribose as raw materials through condensation, deacetylation, and phosphorylation (see Chem.Commun.1999, 729-730), but there ...

Claims

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Application Information

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IPC IPC(8): C07H1/00C07H19/048
CPCC07H1/00C07H19/048
Inventor 兰鲲张浩张祥泰
Owner 青岛新通道合成技术有限公司
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