A method for preparing β-nicotinamide mononucleotide and its sodium salt
A nicotinamide nucleotide and mononucleotide technology is applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., which can solve the problems of high cost, high equipment requirements, slow reaction, etc. Improved yield and purity, good reaction selectivity, and easy purification
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0047] Embodiment 1 A method for preparing β-nicotinamide mononucleotide, comprising the following steps in sequence:
[0048] A, esterification reaction, reaction formula is as follows:
[0049]
[0050] Under an ice-water bath, add 87g of pyridine and 290g of nicotinamide ribose to 500mL of acetonitrile, control the temperature at 0-5°C, then slowly drop 281g of diphenyl chlorophosphate into it, and continue the reaction under stirring for about 12 Hours until the reaction is complete (TLC plate to see the disappearance of raw material spots).
[0051] After the reaction, the acetonitrile was recovered by distillation under reduced pressure at 40-45°C to obtain about 630 g of the crude product of nicotinamide ribose diphenyl phosphate, an intermediate of β-nicotinamide ribose, with a yield of 100%, all of which were directly used in the next step reaction.
[0052] B, hydrolysis reaction, reaction formula is as follows:
[0053]
[0054] At room temperature (20°C, t...
Embodiment 2
[0058] Embodiment 2 A method for preparing β-nicotinamide mononucleotide, comprising the following steps in sequence:
[0059] a. Esterification reaction
[0060] Under an ice-water bath, add 150g of pyridine and 500g of nicotinamide ribose to 1000mL of DMF, control the temperature at 0-5°C, and then slowly drop 485g of diphenyl chlorophosphate into it, and continue the reaction for about 12 hours to complete the reaction ( TLC plate to see disappearance of raw material spots).
[0061] After the reaction, the DMF was recovered by distillation under reduced pressure at 40-50°C, and about 1100 g of crude product of nicotinamide ribose diphenyl phosphate, an intermediate of β-nicotinamide ribose, was obtained, with a yield of 100%, all of which were directly used in the next step reaction.
[0062] b. Hydrolysis reaction
[0063] At room temperature, the crude intermediate nicotinamide ribose diphenyl phosphate obtained in the previous step was dissolved in 5000 mL of methano...
Embodiment 3
[0067] Embodiment 3 A method for preparing sodium β-nicotinamide mononucleotide, comprising the following steps in sequence:
[0068] a. Esterification reaction
[0069] Under an ice-water bath, add 150g of pyridine and 500g of nicotinamide ribose to 1000mL of acetonitrile, control the temperature at 0-5°C, then slowly drop 485g of diphenyl chlorophosphate into it, and continue the reaction for about 12 hours after the addition is complete (TLC Click the board to see the raw material point disappear).
[0070] After the reaction, acetonitrile was recovered by distillation under reduced pressure at 40-50°C to obtain about 1100 g of crude product of nicotinamide ribose diphenyl phosphate, an intermediate of β-nicotinamide ribose, with a yield of 100%, all of which were directly used in the next reaction .
[0071] b. Hydrolysis reaction
[0072] At room temperature, the intermediate nicotinamide ribose diphenyl phosphate crude product obtained in the previous step was dissolv...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More 


