Valnemulin hydrochloride hydrate crystal form and preparation method thereof and pharmaceutical composition containing crystal form
A technology of warnemulin hydrochloride and hydrate, which is applied in the field of crystallization of veterinary medicine and chemical engineering, can solve the problems of difficult industrialization of the crystallization process, unexplained no solvate, no improvement in bulk density, etc., and achieves simple operation steps and preparation process, Ease of industrial production and remarkable practicability
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Embodiment 1
[0059] Take 10g of vernimulin hydrochloride raw material, add 30ml of methanol, then add 20ml of purified water, heat up to 40°C to dissolve, keep stirring for 1 hour, then slowly cool down to 5°C, stir and crystallize for 4h, filter; the filter cake is dissolved in 100ml Stir in n-hexane for 6 hours, and filter; the filter cake was vacuum-dried at 30°C to obtain 9.5 g of warnemulin hydrochloride hydrate, with a yield of 95%, a normalized purity of 99.63%, and a water content of 6.9%.
Embodiment 2
[0061] Take 10g of vonemulin hydrochloride crude drug, add 40ml of ethyl acetate, then add 50ml of purified water, heat up to 60°C to dissolve, keep stirring for 1 hour, then slowly cool down to 10°C, stir and crystallize for 8h, filter; the filter cake dissolves Stir in 150ml of n-heptane for 8h, filter; the filter cake was vacuum-dried at 40°C to obtain 9.2g of warnemulin hydrochloride hydrate, the weight yield was 92%, the purity was 98.8%, and the water content was 6.5%.
Embodiment 3
[0063] Take 10g of the crude drug of warnemulin hydrochloride, add 50ml of ethanol, then add 35ml of purified water, heat up to 55°C to dissolve, heat and stir for 1 hour, then slowly cool down to -5°C, stir and crystallize for 10h, filter; filter cake at 35°C After vacuum-drying at ℃ for 12 hours, place it above a saturated potassium nitrate aqueous solution (92.5% RH), and place it for 16 hours to obtain the 2.5 hydrate crystal form of warnemulin hydrochloride, with a water content of 6.8%;
[0064] At a temperature of 40°C, dry for 20 hours to constant weight to obtain the crystalline form of warnemulin hydrochloride 1.5 hydrate, with a water content of 4.6%;
[0065] Continue drying at 60° C. for 20 h to constant weight to obtain 8.9 g of 1.25 hydrate crystal form of warnemulin hydrochloride, with a yield of 89%, an HPLC purity of 98.9%, and a water content of 3.7%.
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