Levoamlodipine mesylate crystal form, preparation method and use thereof
A kind of technology of levamlodipine and methanesulfonic acid, which is applied in the field of medicine and achieves the effect of high purity
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Embodiment 1
[0026] Add 30.6 g of levoamlodipine and 250 mL of ethyl acetate into the reaction flask, stir to dissolve, add 8 g of methanesulfonic acid, and stir at 25° C. for 16 hours. Filtered to obtain 38 g of a white solid. The solid was recrystallized with 200 mL of ethyl acetate, cooled and crystallized, filtered, and dried under vacuum to obtain 31 g of off-white solid. The purity determined by HPLC method is 99.6%. The X-diffraction pattern of this crystal form is shown in figure 1 , See the infrared spectrum figure 2 .
Embodiment 2
[0028] Add 30.6 g of levoamlodipine and 250 mL of methanol to the reaction flask, stir to dissolve, add 8 g of methanesulfonic acid, stir at 25° C. for 16 hours, add 200 mL of ethyl acetate crystals, filter, and vacuum dry to obtain 27 g of off-white solids. The purity determined by HPLC method was 99.9%, and its X-diffraction pattern and infrared pattern were similar to those of Example 1.
Embodiment 3
[0030] Add 30.6 g of levoamlodipine and 150 mL of acetone to the reaction flask, add 8 g of methanesulfonic acid after stirring to dissolve, stir at 25° C. for 16 h, add 200 mL of ethyl acetate crystals, filter, and vacuum dry to obtain 25 g of off-white solid. The purity determined by HPLC method was 99.8%, and its X-diffraction pattern and infrared pattern were similar to those in Example 1.
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