http://rdf.ncbi.nlm.nih.gov/pubchem/patent/CN-105601534-A

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assignee http://rdf.ncbi.nlm.nih.gov/pubchem/patentassignee/MD5_80fdaa0d94f29478467816f48d47639e
classificationCPCInventive http://rdf.ncbi.nlm.nih.gov/pubchem/patentcpc/C07C245-08
classificationIPCInventive http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07C245-08
filingDate 2015-12-23-04:00^^<http://www.w3.org/2001/XMLSchema#date>
inventor http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_0be20f0f2cd2cfe19a93a631f8c6ee8b
publicationDate 2016-05-25-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationNumber CN-105601534-A
titleOfInvention Synthetic method for oxyphenbutazone drug intermediate-4-hydroxyazobenzene
abstract The invention discloses a synthetic method for an oxyphenbutazone drug intermediate-4-hydroxyazobenzene. The method comprises the following steps: (i) adding 300ml of a sulfuric acid solution with a certain concentration into a reaction container equipped with a stirrer, a temperature meter and a drop funnel, controlling the stirring speed to be 100-200rpm, slowly adding 1.2mol of phenylamine, after phenylamine is completely dissolved, cooling the solution to 6-9 DEG C, dropwise adding 1.1mol of potassium bisulfite, performing dissolution in 200-230ml of water to prepare a solution, testing a reaction termination point by using potassium iodide test paper, and generating diazonium salt (3); and (ii) adding 2-2.3L of a potassium carbonate solution with a certain concentration and 1.2mol of phenol into the other container to prepare a potassium phenate solution, slowly adding a diazotization solution obtained in the step (i) at the stirring speed of 100-160rpm, controlling the temperature of the solution to be 16-20 DEG C, after the addition is finished, continuing to react for 30-40 minutes, adding an adjusting solution for maintaining the pH value of the solution to be 8-9, then adding an oxalic acid solution for reducing the pH value to be 2-3, keeping the reaction for 40-50 minutes, performing suction filtration, adding a washing solution, and performing dewatering with a dewatering agent to obtain 4-hydroxyazobenzene.
isCitedBy http://rdf.ncbi.nlm.nih.gov/pubchem/patent/CN-113105357-A
http://rdf.ncbi.nlm.nih.gov/pubchem/patent/CN-113105357-B
priorityDate 2015-12-23-04:00^^<http://www.w3.org/2001/XMLSchema#date>
type http://data.epo.org/linked-data/def/patent/Publication

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