A kind of crystallization method for preparing high-purity and monodisperse I crystal form atorvastatin calcium in two kettles
A monodisperse technology of atorvastatin calcium, applied in organic chemistry methods, organic chemistry, etc., can solve the problems of easy aggregation of particles and difficult purification
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Embodiment example 1
[0104] Dissolving 7 g of atorvastatin calcium raw material in 40 g of anhydrous methanol at a temperature of 20 to 25° C., and the methanol solution obtained after pressure filtration is used as a feed solution for co-current elution and crystallization.
[0105] In crystallizer, adding methanol content is the methanol-water solution of 65wt% as the solution of elution crystallization, and solution gross mass is 40g, is warming up to 65 ℃, drops into 0.6g I crystal form atorvastatin calcium crystallization powder wherein, makes solution When saturation is reached, 0.2 g of I crystal form atorvastatin calcium is added thereto, suspended and transformed for 1 hour as a seed crystal.
[0106] Using the co-current elution method, the material liquid and the anti-solvent pure water are added to the crystallizer at the same time. Each material is divided into two streams and added. The process time is 8 hours. The methanol content of the solvent in the solution is kept constant durin...
Embodiment example 2
[0114] Dissolve 7 g of atorvastatin calcium raw material in 40 g of anhydrous methanol at a temperature of 20-25° C., and press-filter the resulting methanol solution as a feed solution for co-current elution and crystallization.
[0115] In crystallizer, adding methanol content is the methanol-water solution of 50wt% as the solution of elution crystallization, and solution gross mass is 40g, is warming up to 65 ℃, drops into 0.489g I crystal form atorvastatin calcium crystallization powder wherein, makes solution When saturation is reached, 0.2 g of I crystal form atorvastatin calcium is added thereto, suspended and transformed for 1 hour as a seed crystal.
[0116] The methanol feed liquid and the anti-solvent pure water were added to the crystallizer at the same time, and each material was divided into two feeds. The process time was 8 hours, and the methanol content of the solvent in the solution was kept constant during the entire dissolution process.
[0117] The tempera...
Embodiment example 3
[0124] Dissolve 7 g of atorvastatin calcium raw material in 40 g of anhydrous methanol at a temperature of 20-25° C., and press-filter the resulting methanol solution as a feed solution for co-current elution and crystallization.
[0125] In crystallizer, add methanol content and be the methanol-water solution of 40wt% as the solution of elution crystallization, solution gross mass is 40g, be warming up to 65 ℃, drop into 0.3g I crystal form atorvastatin calcium crystallization powder wherein, make solution When saturation is reached, 0.2 g of I crystal form atorvastatin calcium is added thereto, suspended and transformed for 1 hour as a seed crystal.
[0126] Add the methanol feed liquid and pure water to the crystallizer at the same time, each material is divided into two feeds, the process time is 8h, and the methanol content of the solvent in the solution is kept constant during the whole dissolution process.
[0127] Lower the temperature of the solution to normal tempera...
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Abstract
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