http://rdf.ncbi.nlm.nih.gov/pubchem/patent/CN-103012266-B
Outgoing Links
Predicate | Object |
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assignee | http://rdf.ncbi.nlm.nih.gov/pubchem/patentassignee/MD5_078cb8366425c7f7bb46338421d23406 |
classificationIPCInventive | http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07D223-16 |
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 http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_e069914601b8151de5f0eb58911f6a7c http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_0b0ed8688b1febdee564700ded77b48e http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_c734fa68ea0a0d3c2d87992b4c60158e http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_5fa6203fe476364a10912ca81044462a http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_c4d42aa05f7d30bd16181d358fdd4e77 http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_83d63602cf768fc52f3e7b670e835d1a |
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> |
type | http://data.epo.org/linked-data/def/patent/Publication |
Incoming Links
Total number of triples: 80.