Synthesis method of beta-nicotinamide mononucleotide
A single nucleotide and synthesis method technology, applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., can solve problems such as low efficiency and cumbersome operation, achieve high operation efficiency, ensure high yield, The effect of short reaction times
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Embodiment 1
[0035] Embodiment 1: as figure 1 , a synthetic method of β-nicotinamide mononucleotide, the specific steps are as follows:
[0036] S1, add 60g of nicotinamide, 500mL of hexamethyldisilamine and 3.3g of ammonium sulfate into the reaction kettle, mix and stir for 5min, heat up to 117°C, and reflux for 6h;
[0037] S2, add 500mL of dichloromethane and 160g of tetraacetyl ribose into the reaction kettle, add 70mL of tin tetrachloride, heat to 50°C and react for 1.5h, cool to 0°C, add 20mL of methanol to react for 30min;
[0038] S3, add 1000mL of methanol into the above reaction kettle, cool to -8°C, add 60mL of n-propylamine and react for 20h to obtain a reaction solution containing nicotinamide riboside;
[0039] S4, add 300mL trimethyl phosphate into the above reaction kettle, cool to 0°C, add 26.8mL phosphorus oxychloride under the protection of nitrogen, and react at constant temperature for 10h;
[0040] S5, pour the reaction solution obtained in the above steps into rapi...
Embodiment 2
[0042] Embodiment 2: as figure 1 , a synthetic method of β-nicotinamide mononucleotide, the specific steps are as follows:
[0043] S1, add 122g of nicotinamide, 1L of hexamethyldisilamine and 7g of ammonium sulfate into the reaction kettle, mix and stir for 5 minutes, heat up to 117°C, and reflux for 6 hours;
[0044] S2, add 1L of dichloromethane and 315g of tetraacetyl ribose into the reaction kettle, add 150mL of tin tetrachloride, heat to 50°C and react for 1.5h, cool to 0°C, add 40mL of methanol to react for 30min;
[0045] S3, add 2L of methanol into the above reaction kettle, cool to -8°C, add 120mL of n-propylamine and react for 20h to obtain a reaction solution containing nicotinamide riboside;
[0046] S4, add 600mL trimethyl phosphate into the above reaction kettle, cool to 0°C, add 52mL phosphorus oxychloride under the protection of nitrogen, and react at constant temperature for 10h;
[0047] S5, pour the reaction solution obtained in the above steps into rapid...
Embodiment 3
[0049] Embodiment 3: as figure 1 , a synthetic method of β-nicotinamide mononucleotide, the specific steps are as follows:
[0050] S1, add 60g of nicotinamide, 500mL of hexamethyldisilamine and 3.3g of ammonium sulfate into the reaction kettle, mix and stir for 5min, heat up to 125°C, and reflux for 8h;
[0051] S2, add 500mL of dichloromethane and 160g of tetraacetyl ribose into the reaction kettle, add 70mL of tin tetrachloride, heat to 55°C and react for 1.5h, cool to 0°C, add 20mL of methanol to react for 45min;
[0052] S3, add 1000mL of methanol into the above reaction kettle, cool to -5°C, add 60mL of n-propylamine and react for 22h to obtain a reaction solution containing nicotinamide riboside;
[0053] S4, add 300mL trimethyl phosphate into the above reaction kettle, cool to 0°C, add 26.8mL phosphorus oxychloride under the protection of nitrogen, and react at constant temperature for 12h;
[0054] S5, pour the reaction solution obtained in the above steps into rapidl...
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