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filingDate 2021-12-20-04:00^^<http://www.w3.org/2001/XMLSchema#date>
inventor http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_535cf09762d6226019df8a7b08d5ee7d
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publicationDate 2022-01-14-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationNumber CN-113929592-A
titleOfInvention A kind of preparation method of doxycycline intermediate
abstract The invention relates to the technical field of veterinary drugs, in particular to a method for preparing a doxycycline intermediate, comprising the following steps: (1) mixing metacycline p-toluenesulfonate and absolute ethanol in proportion, and then adding concentrated Hydrochloric acid, the temperature of the reaction system after stirring and mixing is controlled at 10-35°C; (2) Zinc borohydride solution is added dropwise to the reaction system in step (1), and the heat preservation reaction time is controlled at 2-5h, and the obtained feed liquid is used for later use (3) under the condition of 20-30 ℃, the sulfosalicylic acid aqueous solution and the feed liquid in the step (2) are added dropwise to the feed liquid of the step (2) according to the mass ratio of 0.7-1.5:1, After 4-6 hours of incubation reaction, the temperature was lowered to 0-10 °C, and the doxycycline sulfosalicylate was obtained by filtration. By using the preparation method, the conversion rate and selectivity of raw materials and the yield of doxycycline p-toluenesulfonate are improved, and the reduction cost and the safety risk in the reaction process are reduced.
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