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申请号:202010013704.8 公开号:CN111153953A 主分类号:C07H19/048
申请人:【中文】杭州洁汉化工有限公司【EN】Hangzhou Jiehan Chemical Co., Ltd 申请日:2020.01.07 公开日:2020.05.15
摘要:【中文】本发明公开了一种烟酰胺核糖氯化物的高效合成方法,采用核糖环羟基上具有乙酰基保护的化合物A作为原料,直接进行氧化得到化合物B,再脱去乙酰基得到烟酰胺核糖氯化物;包括如下合成步骤:1)在高压釜中加入化合物A,并加入氯化铵、铂碳和乙醇,通入氧气,室温搅拌至反应完成;2)过滤回收铂碳,减压脱除溶剂后加入无水乙醇,冷却析出白色固体后过滤,干燥得到化合物B;3)在三口瓶中加入化合物B并溶于乙醇,通入氨气后保温,反应完后将反应液冷却至析出固体,过滤,干燥得到烟酰胺核糖氯化物。本发明采用乙酰基保护核糖羟基后再进行氧化,减少了副反应,使氧化收率大大提高,同时采用氧气加压的方式进行氧化反应,大大提高了反应效率。 【EN】The invention discloses a high-efficiency synthesis method of nicotinamide riboside chloride, which adopts a compound A with acetyl protection on ribose ring hydroxyl as a raw material, directly oxidizes the compound A to obtain a compound B, and deacetylates the compound B to obtain the nicotinamide riboside chloride; comprises the following synthesis steps: 1) adding the compound A into the high-pressure kettle, adding ammonium chloride, platinum carbon and ethanol, introducing oxygen, and stirring at room temperature until the reaction is finished; 2) filtering to recover platinum carbon, removing the solvent under reduced pressure, adding absolute ethyl alcohol, cooling to separate out white solid, filtering, and drying to obtain a compound B; 3) and adding the compound B into a three-neck flask, dissolving the compound B in ethanol, introducing ammonia gas, keeping the temperature, cooling the reaction solution after the reaction is finished to separate out a solid, filtering, and drying to obtain the nicotinamide riboside chloride. According to the invention, the acetyl is adopted to protect the ribose hydroxyl and then oxidized, so that side reactions are reduced, the oxidation yield is greatly improved, and meanwhile, the oxidation reaction is carried out in an oxygen pressurization mode, so that the reaction efficiency is greatly improved.
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