Method for preparing niacinamide nucleoside salt

A technology for nicotinamide nucleoside salt and nicotinamide nucleoside trifluoromethanesulfonate, which is applied in the field of preparing nicotinamide nucleoside salt, can solve the problems of reduced total yield, unsuitability for industrial production, increased reduction reaction and the like, and achieves the Simple operation, suitable for large-scale production, avoid the effect of degradation

Inactive Publication Date: 2018-11-09
张洪喜
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This chemical deionization avoids the ion exchange process, but increases the oxidation and reduction reactions, the steps increase, and the total yield decreases below 20%, which is also not suitable for industrial production.

Method used

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  • Method for preparing niacinamide nucleoside salt
  • Method for preparing niacinamide nucleoside salt

Examples

Experimental program
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Embodiment 1-A

[0033] Embodiment 1-A: Preparation of nicotinamide nucleoside chloride

[0034]A mixture of triacetyl nicotinamide nucleoside trifluoromethanesulfonate (53g, 0.1mol) and methanol (50ml) was added dropwise to 7N ammonia methanol solution (100ml) at -10°C, and kept stirring at -10°C for 24h , after the sampling detection reaction finishes, control -10 ℃ and drop 28% hydrogen chloride methanol solution (100ml) to neutralize, filter to remove ammonium chloride, filtrate control -10 ℃ drop 28% hydrogen chloride methanol solution (40ml) to replace ions, Add ethyl acetate (1000ml) dropwise to crystallize, keep stirring at -10°C for 1h, and filter to obtain the crude product.

[0035] Add methanol (100ml) to the crude product to cool down to -10°C, add dropwise 28% methanolic hydrogen chloride solution (6ml), beat for 4 hours, and filter to obtain a beating solid; % hydrogen chloride methanol solution (3ml), beating for 4h, the beating temperature is -5°C, the wet product was obtaine...

Embodiment 1-B

[0036] Example 1-B: Preparation of nicotinamide nucleoside chloride

[0037] A mixture of triacetyl nicotinamide nucleoside trifluoromethanesulfonate (53g, 0.1mol) and methanol (50ml) was added dropwise to 30% sodium methoxide methanol solution (27g, 0.15mol) at -7°C, and kept at -7 Stir the reaction at ℃ for 1 hour, and after the reaction is completed by sampling and testing, add 28% methanolic hydrogen chloride solution (25ml) dropwise at -4°C to neutralize, filter to remove sodium chloride, and add 28% methanolic hydrogenchloride solution (25ml) dropwise to the filtrate at -4°C ) to replace ions, dropwise added ethyl acetate (500ml) to crystallize, kept stirring at -7°C for 1h, and filtered to obtain a crude product.

[0038] Add methanol (100ml) to the crude product to cool down to -7°C, add dropwise 28% methanolic hydrogen chloride solution (6ml), beat for 4 hours, and filter to obtain a beating solid; % hydrogen chloride methanol solution (3ml), beating for 4h, the beat...

Embodiment 1-C

[0039] Example 1-C: Preparation of nicotinamide nucleoside chloride

[0040] A mixture of triacetyl nicotinamide nucleoside trifluoromethanesulfonate (53g, 0.1mol) and methanol (50ml) was added dropwise to 7N ammonia methanol solution (100ml) at -8°C, and the mixed solution was kept at -9°C , stirring and reacting for 24 hours, sampling and testing the remaining 1% of the raw material, the reaction is over, the temperature of the solution is controlled at -7°C, and concentrated sulfuric acid (29g, 0.3mol) is added dropwise to neutralize, the ammonium sulfate is removed by filtration, and the filtrate is controlled at -8°C and 28 % methanolic hydrogen chloride solution (40ml) to replace ions, dropwise added ethyl acetate (600ml) to crystallize, keep stirring at -9°C for 1h, and filter to obtain the crude product.

[0041] Add methanol (100ml) to the crude product and cool down to -8°C, add dropwise 28% hydrogen chloride methanol solution (6ml), beat for 4 hours, and filter to o...

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Abstract

The invention relates to a method for preparing niacinamide nucleoside salt. The method comprises the following steps: replacing ions by niacinamide nucleoside trifluoromethane sulfonate prepared by deacetylation of triacetyl niacinamide nucleoside trifluoromethane in an organic solvent with acids, crystallizing to separate out a crude product, and pulping, thereby obtaining the corresponding niacinamide nucleoside salt. The ion replacement process in the invention overcomes the defects of chemical methods and extraction methods, and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of nutritional supplements, and in particular relates to a method for preparing nicotinamide nucleoside salt. Background technique [0002] Nicotinamide nucleoside and nicotinamide mononucleotide are metabolites of nicotinamide adenine dinucleotide, which are potential natural nutritional supplements. [0003] CN201580040316 uses nicotinamide and tetraacetyl ribose as raw materials, generates triacetyl nicotinamide nucleoside trifluoromethanesulfonate under the catalysis of trimethylsilyl trifluoromethanesulfonate, and then uses sodium methoxide to remove the acetyl group to obtain nicotinamide Amide nucleoside triflate. To replace the triflate anion with safer chloride or other anions, an aqueous solution containing nicotinamide nucleoside, sodium chloride, and alkali metal triflate was extracted with THF. This ion-exchange method avoids the ion-exchange resin method, but needs to remove water and sodium ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H19/048C07H1/06
CPCC07H1/06C07H19/048
Inventor 张洪喜
Owner 张洪喜
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