http://rdf.ncbi.nlm.nih.gov/pubchem/patent/CN-106431875-A
Outgoing Links
Predicate | Object |
---|---|
assignee | http://rdf.ncbi.nlm.nih.gov/pubchem/patentassignee/MD5_ac3bf74f2e240d94a4ca2f04e6708d2d |
classificationCPCInventive | http://rdf.ncbi.nlm.nih.gov/pubchem/patentcpc/C07C67-343 http://rdf.ncbi.nlm.nih.gov/pubchem/patentcpc/C07C45-676 |
classificationIPCInventive | http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07C49-213 http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07C69-738 http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07C45-65 http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07C67-343 |
filingDate | 2016-09-18-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
inventor | http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_12607d5efbcbf9d16b38506c80a6d6ae |
publicationDate | 2017-02-22-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
publicationNumber | CN-106431875-A |
titleOfInvention | Method for synthesizing antitussone medicine intermediate benzyl acetone |
abstract | A method for synthesizing an antitussone medicine intermediate benzyl acetone includes the following steps that 320 ml of cyclohexane is added into a reaction container provided with a stirrer, a reflux condenser, a dropping funnel and a thermometer, 1.3 mol of stannous chloride is added in batches, 2.3 mol of ethyl acetoacetate is added, the stirring speed is controlled to be 130-160 rpm, reaction is conducted for 60-90 min, the temperature of the solution is raised to 65-70 DEG C, reflux is conducted for 3-5 h, 2.6-2.8 mol of benzyl amine (3) is dropwise added, dropping time is controlled to be 3-4 h, and a reflux reaction is conducted for 3-4 h to produce an intermediate product; the temperature of the solution is reduced to 10-15 DEG C, 330 mol of potassium bisulfite is added, and reflux continues for 4-5 h to generate an oily product; oxalic acid is added to adjust the pH of the solution at 4-5, reflux continues for 4-6 h, reduced pressure distillation is carried out, fractions at 95-105 DEG C are collected, washed with a saline solution and acetonitrile and re-crystallized in nitromethane, and crystal benzyl acetone is obtained. |
priorityDate | 2015-12-24-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
type | http://data.epo.org/linked-data/def/patent/Publication |
Incoming Links
Total number of triples: 47.