Citicoline drug preparation and its new application of consciousness disorder in acute stage of cerebral infarction
A technology for citicoline and citicoline sodium, which is applied in the field of preparation of citicoline, can solve the problems of incomplete reaction of raw materials, side reactions, and high cost, and can solve the problems of post-processing difficulties and reaction conditions. Mild, reduced complexity effects
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[0046] Specifically, the present invention provides a kind of preparation method of citicoline sodium or its composition, described method comprises the following steps:
[0047] Step 1: Combine 5'-cytidylic acid and phosphorylcholine chloride (C 5 h 15 ClNO 4 P) Disperse in an aprotic organic solvent, add 1-propyl phosphoric acid cyclic anhydride (T 3 P) reaction, filter out the insolubles in the reaction solution, collect the filtrate;
[0048] Step 2: cooling the filtrate in step 1, separating out crystals, and filtering to obtain citicoline;
[0049] Step 3: Citicoline acid reacts with sodium base / salt to generate citicoline sodium, which is citicoline.
[0050] The synthetic route schematic diagram of the present invention is as follows:
[0051]
[0052] In step 1, the added 1-propyl phosphoric acid cyclic anhydride acts as a condensing agent to condense the 5'-cytidylic acid and phosphorylcholine chloride dispersed in the aprotic organic solvent. The activation...
Embodiment 1
[0129] Preparation of Citicoline Sodium:
[0130] Add 50g of 5'-cytidylic acid, 500ml of acetonitrile, and 36g of phosphorylcholine chloride into the reaction flask, start stirring, add 52g of 1-propylphosphoric acid cyclic anhydride at a rate of 2.0ml / min at 25°C, and stir after adding After 1 hour, the temperature was raised to reflux of the reaction system, and after 3 hours of reflux reaction, the temperature of the reaction system was lowered to 55°C and filtered while hot, and the filtrate was collected;
[0131] The filtrate was naturally cooled to 25°C, a large amount of crystals were precipitated, and citicoline acid was obtained by filtration, and the filtrate was applied to the next batch;
[0132] Dissolve the collected citicoline acid in 1000ml of purified water, raise the temperature to 35°C and stir to dissolve, then add sodium bicarbonate to adjust the pH value to 7.5. Cool the solution to 10°C, keep it warm for 45 minutes, and collect citicoline sodium by fil...
Embodiment 2
[0136] Preparation of Citicoline Sodium:
[0137] Add 50 g of 5'-cytidylic acid, 500 ml of acetonitrile, and 34.5 g of phosphorylcholine chloride into the reaction flask, start stirring, add 49.5 g of 1-propyl phosphoric acid cyclic anhydride at a rate of 1.5 ml / min at 30°C, and add After stirring for 0.75 hours, the temperature was raised to reflux of the reaction system, and after 5 hours of reflux reaction, the temperature of the reaction system was lowered to 60°C and filtered while it was hot, and the filtrate was collected;
[0138] The filtrate was cooled to 15°C, a large number of crystals were precipitated, and citicoline acid was obtained by filtration, and the filtrate was applied to the next batch;
[0139] Dissolve the collected citicoline acid in 1000ml of purified water, raise the temperature to 40°C and stir to dissolve, then add sodium bicarbonate to adjust the pH value to 7. Cool the solution to 10°C, keep it warm for 60 minutes, and collect citicoline sodiu...
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