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filingDate 2020-06-30-04:00^^<http://www.w3.org/2001/XMLSchema#date>
inventor http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_d1f2affb524225e1ba364dfe30aca6ea
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publicationDate 2020-10-09-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationNumber CN-111748004-A
titleOfInvention A kind of crystal form of high-purity dapagliflozin intermediate and preparation method thereof
abstract The invention discloses a crystal form of a high-purity dapagliflozin intermediate and a preparation method thereof. -C8 hydrocarbon mixed solution crystallization, specifically, the compound of formula 1 is dissolved in methanol and C5-C8 hydrocarbon mixed solution, the concentration is about 0.01g/ml~2.0g/ml, preferably 0.1g/ml~1.0g/ml , more preferably 0.20g/ml~0.80g/ml, stir and crystallize the mixed solution of n-methanol and C5-C8 hydrocarbons containing the compound of the above formula 1, filter, and dry under reduced pressure to obtain the high-purity compound of formula 1, the formula 1 of the present invention The crystal form of the compound not only has high purity, but also has good stability, which can effectively separate and purify the dapagliflozin intermediate from the reaction solution, remove impurities generated during the reaction, and make the purity of the dapagliflozin intermediate from 75% to 90%. % is increased to more than 99.5%; the preparation method has simple and controllable technological operation, good reproducibility, easy realization of industrialized production, improved efficiency and reduced production cost.
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