http://rdf.ncbi.nlm.nih.gov/pubchem/patent/CN-102690211-B
Outgoing Links
Predicate | Object |
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classificationIPCInventive | http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07C231-12 http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07C233-81 |
filingDate | 2012-06-05-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
grantDate | 2015-12-09-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
publicationDate | 2015-12-09-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
publicationNumber | CN-102690211-B |
titleOfInvention | The preparation method of tolvaptan intermediate |
abstract | The present invention relates to a kind of preparation method of tolvaptan intermediate.With 2-methyl-4-nitrobenzoic acid for starting raw material, under catalyst action, generate 2-methyl-4-nitrobenzoyl acid esters with alcohols reaction, then be that hydrogen donor is obtained by reacting 2-methyl-PABA ester compound under the catalysis of palladium charcoal with ammonium formiate; Gained ester compound is reacted with o-methyl-benzene formyl chloride under alkaline condition, generate 2-methyl-4-N-(2-toluyl) benzoic ether, again under water existence condition, add alkali and catalyzer is hydrolyzed, and with organic reagent extraction 1 ~ 2 water layer, after layering, collect water layer solution, regulate water layer pH value of solution=5 ~ 6 to separate out solid, the elimination aqueous solution, the solid excess of gained dries and is target product.The present invention not only increases quality product and yield, also simplify the treatment process of intermediate, for suitability for industrialized production provides a kind of processing method of simple possible. |
priorityDate | 2012-06-05-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
type | http://data.epo.org/linked-data/def/patent/Publication |
Incoming Links
Total number of triples: 104.