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filingDate 2012-11-23-04:00^^<http://www.w3.org/2001/XMLSchema#date>
grantDate 2014-07-23-04:00^^<http://www.w3.org/2001/XMLSchema#date>
inventor http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_ab17765e0a67fc1d09bd370779f2055d
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publicationDate 2014-07-23-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationNumber CN-103012266-B
titleOfInvention Preparation method of 7-chloro-5-oxo-2,3,4,5-tetrahydro-1H-1-benzazepine
abstract The invention relates to a preparation method of 7-chloro-5-oxo-2,3,4,5-tetrahydro-1H-1-benzazepine, which is an important intermediate for preparing arginine vasopressin V2 receptor antagonist Tolvaptan. The preparation method comprises the following steps: with methyl 2-amido-5-chlorobenzoate and ethyl 4-bromobutyrate as starting raw materials, reacting at a low temperature under the effect of an acid binding agent to generate secondary amine first, then carrying out Dieckman condensation reaction at a raised temperature to generate an intermediate mixture III, and finally carrying out hydrolysis to obtain the target compound 7-chloro-5-oxo-2,3,4,5-tetrahydro-1H-1-benzazepine. Compared with the existing method, the method provided by the invention has the advantages that the reaction steps are reduced, the two-step reaction is simplified to one-step reaction through temperature control, so the operation is simple, the processing is convenient, the product purity is high, and the yield is also greatly improved, thus the production cost can be reduced, and the benefits are increased.
priorityDate 2012-11-23-04:00^^<http://www.w3.org/2001/XMLSchema#date>
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