Refining method of disodium phosphocreatine
A technology of creatine phosphate disodium salt and creatine phosphate disodium salt is applied in the refining field of creatine phosphate disodium salt, can solve the problems of poor timeliness, long crystallization time, long process time, etc., and can meet the requirements of industrialized large-scale production , the conditions are mild and easy to control, and the process method is simple.
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example 1
[0030] Take 15.0 g of crude creatine phosphate disodium (purity 92.1%), add 15 ml of water at room temperature and stir for 10 minutes to dissolve, filter, and add 45 ml of ethanol to the filtrate with stirring to precipitate a large amount of oil; let it stand for 1 hour and separate Remove the supernatant liquid, add 30ml methanol to the oily substance with stirring, a large amount of crystals will be precipitated, be slurried and crystallized for 1 hour, and then filtered; the filter cake is transferred to the reaction flask, 30ml ethanol is added and washed for 1 hour, filtered, the filter cake is at 40 After drying under reduced pressure at ~45°C, 13.0 g of creatine phosphate disodium salt tetrahydrate compound was obtained, with a purity of 99.1% and a yield of 86.7%.
example 2
[0032] Take 15.0 g of creatine disodium phosphate (purity 88.5%), add 75ml of water at room temperature and stir for 10 minutes to dissolve, filter, add 225ml of ethanol to the filtrate with stirring, and precipitate a large amount of oil; let it stand for 1 hour and separate Remove the supernatant liquid, add 75ml of methanol to the oily substance under stirring to precipitate a large number of crystals, beating and crystallizing for 1 hour, filter; transfer the filter cake to the reaction flask, add 75ml of ethanol, stir and wash for 1 hour, filter, filter the cake at 40~ After drying under reduced pressure at 45°C, 10.5 g of creatine phosphate disodium salt tetrahydrate compound was obtained, with a purity of 99.2% and a yield of 70.0%.
example 3
[0034] Take 15.0 grams of crude creatine phosphate disodium (purity 92.1%), add 15ml of water at room temperature and stir for 10 minutes to dissolve, filter, and add 45ml of isopropanol to the filtrate with stirring to precipitate a large amount of oil; let it stand for 1 hour Afterwards, the supernatant liquid was separated and removed. Under stirring, 30ml of methanol was added dropwise to the oily substance to precipitate a large number of crystals, which were slurried for 1 hour and filtered; the filter cake was transferred to the reaction flask, and 30ml of isopropanol was added and washed for 1 hour, filtered, filtered After the cake was dried under reduced pressure at 40-45°C, 13.5 g of creatine phosphate disodium salt tetrahydrate compound was obtained, with a purity of 99.0% and a yield of 90.0%.
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