Atorvastatin calcium compound
A technology of atorvastatin calcium and trihydrate, which is applied in the field of medicine and can solve the problems of large number of impurities, high total amount of impurities, difficult to repeat crystal form and the like of atorvastatin calcium trihydrate.
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Embodiment 1
[0044] In a 100L reaction kettle, add 6 kg of atorvastatin calcium trihydrate (purity 98.06%, HPLC) and 65 L of acetone-acetonitrile-ammonia = 9:1:0.5 mixture, heat to 50°C-55°C , keep warm for 20 minutes, and filter while hot. The filtrate was kept at 35°C-38°C for 1.5 hours; then naturally cooled to room temperature and held for 2.5 hours, the precipitated crystals were filtered and dried naturally at room temperature to obtain 5.71 kg of white crystals with a purity of 99.91%. The solvent residue test met the requirements. The moisture measured by Karl Fischer method is 4.45%.
[0045] The X-ray diffraction pattern of the crystal is shown in figure 1 . Instrument model and measurement conditions: Rigaku D / max 2500 diffractometer; CuKa 40Kv 100mA; 2θ scanning range: 0-50 ° .
Embodiment 2
[0047] In a 100L reactor, add 6 kg of atorvastatin calcium trihydrate (purity 98.06%, HPLC) and 60 L of acetone-acetonitrile-ammonia = 9:0.8:0.3 mixture, heat to 50°C-53°C , keep warm for 20 minutes, and filter while hot. The filtrate was kept at 35°C-36°C for 1 hour; then naturally cooled to room temperature and held for 2 hours, the precipitated crystals were filtered and dried naturally at room temperature to obtain 5.56 kg of white crystals with a purity of 99.92%. The solvent residue test met the requirements. The moisture measured by Karl Fischer method is 4.44%.
[0048] The X-ray diffraction figure that measures is the same as the X-ray diffraction figure of embodiment 1 ( figure 1 ).
Embodiment 3
[0050] In a 100L reactor, add 6 kg of atorvastatin calcium trihydrate (purity 98.06%, HPLC) and 70 L of acetone-acetonitrile-ammonia = 9:0.5:0.7 mixture, heat to 52°C-54°C , keep warm for 20 minutes, and filter while hot. The filtrate was kept at 37°C-38°C for 2 hours; then naturally cooled to room temperature and kept for 3 hours, the precipitated crystals were filtered and dried naturally at room temperature to obtain 5.66 kg of white crystals with a purity of 99.92%, and the solvent residue test met the requirements. The moisture measured by Karl Fischer method is 4.47%.
[0051] The X-ray diffraction figure that measures is the same as the X-ray diffraction figure of embodiment 1 ( figure 1 ).
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