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filingDate 2020-09-08-04:00^^<http://www.w3.org/2001/XMLSchema#date>
inventor http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_13bfee3a592729f303df2ec33e9c9080
publicationDate 2020-11-06-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationNumber CN-111892478-A
titleOfInvention A kind of synthetic method of saxagliptin intermediate
abstract A method for synthesizing a saxagliptin intermediate, using the following techniques: (1) substitution reaction of adamantane (compound 1) and liquid bromine under the catalysis of aluminum tribromide and boron tribromide to obtain compound 2; ( 2) compound 2 and diethyl acetamidomalonate are dissolved in sherwood oil, react under the effect of sodium ethylate, then add L-arginine for backflow reaction 8 hours in the acidic solution, hydrolysis and decarboxylation form compound 3; (3) Compound 3 is hydrolyzed to form compound 4 by stirring and refluxing for 8 hours in the presence of a base; (4) Compound 4 is reacted with Boc acid anhydride at room temperature for 12 hours to obtain intermediate saxagliptin body. The raw materials and reagents used in the invention are cheap and easy to obtain, the reaction operation is simple, the reaction conditions are mild, the yield is high, the quality is excellent, and the final product of the split can reach 99% ee value, which meets the requirements of pharmaceutical intermediates.
priorityDate 2020-09-08-04:00^^<http://www.w3.org/2001/XMLSchema#date>
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