http://rdf.ncbi.nlm.nih.gov/pubchem/patent/CN-108863846-B
Outgoing Links
Predicate | Object |
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classificationCPCInventive | http://rdf.ncbi.nlm.nih.gov/pubchem/patentcpc/C07C253-30 |
classificationIPCInventive | http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07C255-60 http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07C253-30 |
filingDate | 2017-05-09-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
grantDate | 2020-11-06-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
publicationDate | 2020-11-06-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
publicationNumber | CN-108863846-B |
titleOfInvention | Preparation method of intermediate of lodoxylamine tromethamine |
abstract | The invention belongs to the technical field of pharmaceutical chemicals, and particularly discloses a preparation method of a lodoxylamine tromethamine intermediate, namely lodoxylamine, which comprises the following steps of (1) dissolving 3, 5-diamino-4-chlorobenzonitrile in an organic solvent to form a solution A; (2) dissolving oxalyl chloride in an organic solvent to form a solution B; (3) slowly dripping the solution A into the solution B, controlling the temperature of the reaction solution to be between 20 ℃ below zero and 0 ℃ in the dripping process, slowly dripping a certain amount of ice water into the reaction solution after the reaction is finished, continuously stirring for 0.5 to 1 hour after the dripping is finished, performing suction filtration, and drying the obtained filter cake to obtain the lodoxylamine. The method has the advantages of few reaction steps, more convenience for operation, greatly improved yield, high purity of the product, namely the lodoxylamine, of more than 90 percent, fewer related impurities, high purity of the product, high HPLC (high performance liquid chromatography) purity of more than 99.5 percent, and great significance for synthesis of the lodoxylamine tromethamine medicament. |
priorityDate | 2017-05-09-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
type | http://data.epo.org/linked-data/def/patent/Publication |
Incoming Links
Total number of triples: 33.