Preparation method of choline alfoscerate crystal
A technology of choline alfoscerate and crystal, which is applied in the field of preparation of choline alfoscerate, can solve the problems such as the decrease of the purity of choline alfoscerate, weakening of the health-care performance and medicinal value of choline alfoscerate
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[0015] The invention provides a kind of preparation method of choline alfoscerate crystal, and this preparation method comprises:
[0016] (1) mixing choline alfoscerate and alcohol to prepare mixture M1;
[0017] (2) Mix the mixture M1 and sulfate, perform the first filtration after cooling and take the filtrate to obtain the mixture M2;
[0018] (3) carrying out the first concentration of the mixture M2 to obtain the mixture M3;
[0019] (4) mixing the mixture M3 with an organic solvent and performing a second concentration to obtain a mixture M4;
[0020] (5) crystallize after mixing ethyl acetate and the mixture M4 and perform second filtration to obtain crystal M5;
[0021] (6) post-processing the crystal M5 to obtain choline alfoscerate crystals.
[0022] In the present invention, the specific type of alcohol can be selected in a wide range, and can be selected from one or more of ethanol, methanol and ethylene glycol. In order to fully dissolve choline alfoscerate, p...
Embodiment 1
[0039] (1) Mix and stir choline alfoscerate and ethanol (100:500 by weight) at 38°C for 60 minutes to prepare mixture M1;
[0040] (2) Mix the mixture M1 and sodium sulfate (100:35 by weight), cool at 27°C for 60 minutes, then perform the first filtration and take the filtrate to obtain the mixture M2;
[0041] (3) Under the conditions of 48°C and 70KPa, the mixture M2 was first concentrated for 1.5h to obtain the mixture M3;
[0042] (4) Mix the mixture M3 and ethanol (100:60 by weight) and conduct the second concentration at 35° C. for 2 h to prepare the mixture M4;
[0043] (5) At 48°C, mix ethyl acetate and the mixture M4 (50:100 by weight) under the condition of 70KPa, crystallize after mixing, and perform second filtration to obtain crystal M5;
[0044] (6) Drying the crystal M5 at 0.7 MPa for 2 hours at 40° C. to obtain choline alfoscerate crystal A1.
Embodiment 2
[0046] (1) At 37°C, mix and stir choline alfoscerate and methanol (100:450 by weight) for 80 minutes to prepare mixture M1;
[0047] (2) Mix the mixture M1 and potassium sulfate (weight ratio: 100:30), cool at 25°C for 50 minutes, then perform the first filtration and take the filtrate to obtain the mixture M2;
[0048] (3) At 45°C and 80KPa, the mixture M2 was first concentrated for 1 hour to obtain the mixture M3;
[0049] (4) Mix the mixture M3 and acetone (100:50 by weight) and conduct the second concentration at 40° C. for 1 h to prepare the mixture M4;
[0050] (5) At 45°C, mix ethyl acetate and the mixture M4 (40:100 by weight) under the condition of 60KPa, crystallize and perform second filtration to obtain crystal M5;
[0051] (6) Drying the crystal M5 at 0.6 MPa for 1 h at 38° C. to obtain choline alfoscerate crystal A2.
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