A kind of refining method of gabexate mesylate
A technology of gabexate mesylate and its refining method, which is applied in the fields of chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as increased risk of medication, prone to hydrolysis, poor clarity, etc. The effects of small reaction, improved pH value and clarity, and simple operation
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Embodiment 1
[0038] Resin pretreatment: Take 300g of commercially available macroporous adsorption resin AB-8 and 900mL of an appropriate solvent, stir and beat at room temperature for 2 hours; filter with suction, rinse the filter cake with 300mL of the corresponding solvent; put it in a decompression drying box for 35- Dry under reduced pressure at 45°C for 6 hours to obtain the pretreated macroporous adsorption resin AB-8.
[0039] Solvent handling Amount of macroporous resin after treatment yield acetone 90.00g 30.0％ Acetonitrile 93.10g 31.0％ Tetrahydrofuran 95.40g 31.8％ ethanol 95.70g 31.9％
Embodiment 2
[0041] Add 10g of crude gabexate mesylate and 50mL of acetone to the reaction flask, raise the temperature to 55°C, and stir for 0.5 hours; add 0.1g of triethylamine and 2g of pretreated AB-8 to the reaction system, beat at 55°C for 2 hour; through a 0.2 micron membrane filter, the filtrate was stirred and crystallized at 25°C, and slurried for 0.5 hour; suction filtered, and the filter cake was dried under reduced pressure at 35°C for 8 hours to obtain the refined product of Gabexate mesylate, a white powder, The yield was 71.0%, and the purity was 99.25%. Its pH was measured to be 5.2, and its clarity in chloroform was measured, and the result was shallower than No. 0.5 turbidity standard solution.
Embodiment 3
[0043] Add 10g of crude gabexate mesylate and 50mL of acetone to the reaction flask, raise the temperature to 55°C, and stir for 0.5 hours; add 0.15g of triethylamine and 2g of pretreated AB-8 to the reaction system, beat at 55°C for 2 hour; through a 0.2 micron membrane filter, the filtrate was stirred and crystallized at 25°C, and slurried for 0.5 hour; suction filtered, and the filter cake was dried under reduced pressure at 35°C for 8 hours to obtain the refined product of Gabexate mesylate, a white powder, The yield was 69.0%, and the purity was 99.17%. Its pH was measured to be 5.2, and its clarity in chloroform was measured, and the result was shallower than No. 0.5 turbidity standard solution.
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