Method for preparing citicoline sodium by utilizing oxalyl chloride
A technology of citicoline sodium and oxalyl chloride, applied in the field of biopharmaceuticals, can solve the problems of high synthesis price, only one-time use, a large amount of yeast, etc., and achieves a good atomic economy, simple operation process, and improved yield. Effect
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[0031] Put 2.58 kg of calcium phosphoric acid choline chloride into a 50L neutralization reaction pot, add 10L of pyridine and 0.5L of benzene, heat to reflux, and separate the water with a water separator. Cool to room temperature.
[0032] Add 0.8 kg of oxalyl chloride to the reaction pot, react for 1 hour, add 10 L of THF solution containing 2.5 kg of cytidylic acid, and stir and react at room temperature for 5 hours. The solvent was recovered under reduced pressure.
[0033] The remaining viscous material was added to 5L of a mixed solution containing 10% sodium hydroxide and 10% sodium carbonate, heated and stirred, and the insoluble matter was filtered off. After adding 60 g of activated carbon to the solution and stirring for 30 min to decolorize, filter. Add 20L of absolute ethanol to the filtrate while stirring and cooling to 0°C, let it stand for 12 hours to precipitate all the solids, and centrifuge to obtain the product. After drying at 100°C, 4.3Kg of solid was...
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