Method for preparing linezolid crystal form I
A technology of linezolid and crystal form, which is applied in the field of producing linezolid crystal form I with high crystal purity and chemical purity, and can solve the problems of low crystal form purity and unstable process of linezolid crystal form I
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[0050]The present invention provides a method for preparing linezolid crystal form I, wherein the crude product of linezolid used in the present invention may be a crude product containing linezolid crystal form II, said linezolid containing crystal form II The crude product can be prepared by any known method in the art (for example WO02085849A2), and the crude product with the content of linezolid crystal form II ≥ 75% (preferably 75-98%) can also be used.
[0051] Preferably, the preparation method of the linezolid crystal form I comprises the steps of:
[0052] (1) Mix the crude product of linezolid with the first solvent, filter, and collect the filtrate;
[0053] Preferably, the step (1) is: after mixing the crude product of linezolid with the first solvent, stirring at 85-105° C. until the crude product is dissolved, then filtering while hot, and collecting the filtrate.
[0054] Wherein, the weight-to-volume ratio of the crude linezolid to the first solvent is 1:15-1:...
Embodiment 1
[0072] Weigh 20g of linezolid crystal form II (crude product, the crystal form II content is about 82%) and 700ml of DMF-toluene (w / w=10:90) mixed solvent, add it to a 2000ml three-necked flask, the temperature of the solution in the flask A DF-101S collector type constant temperature magnetic stirrer is used for program temperature control (internal temperature is controlled at 95-100°C), and mechanical stirring is used for thorough mixing until the solute is dissolved;
[0073] The solution was filtered while hot and the resulting clear filtrate was transferred to a flask. Adjust the mechanical stirrer so that its stirring rate is 300rpm / min;
[0074] Start the feeding device, dropwise add 560ml of heptane at a rate of 0.6ml / min, after the dropwise addition of heptane is completed, grow the crystal for 10min, slowly cool down to 3-5°C, and continue stirring for 1h in this temperature range;
[0075] The crystal slurry was filtered, and the filter cake was washed with 3×5 mL...
Embodiment 2
[0080] Weigh 18g of linezolid crystal form II (crude product, the content of crystal form II is about 80%) and 540ml of DMF-toluene (w / w=15:85) mixed solvent, add it to a 2000ml three-necked flask, the temperature of the solution in the flask A DF-101S collector type constant temperature magnetic stirrer is used for program temperature control (internal temperature is controlled at 98-102°C), and mechanical stirring is used for thorough mixing until the solute is completely dissolved;
[0081] The solution was filtered while hot and the resulting clear filtrate was transferred to a flask. Adjust the mechanical stirrer so that the stirring rate is 300 rpm / min, and add 0.95 g of seed crystals whose particle size range is 63-75 μm;
[0082] Start the feeding device, add the second solvent heptane 540ml heptane dropwise at a rate of 0.8ml / min, grow the crystal for 10min, slowly cool down to 3-5°C, and continue stirring for 1h in this temperature range;
[0083] The crystal slurry...
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