http://rdf.ncbi.nlm.nih.gov/pubchem/patent/CN-105622329-A
Outgoing Links
Predicate | Object |
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assignee | http://rdf.ncbi.nlm.nih.gov/pubchem/patentassignee/MD5_80fdaa0d94f29478467816f48d47639e |
classificationCPCInventive | http://rdf.ncbi.nlm.nih.gov/pubchem/patentcpc/C07C17-093 http://rdf.ncbi.nlm.nih.gov/pubchem/patentcpc/C07C245-20 |
classificationIPCInventive | http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07C17-093 http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07C25-13 |
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 | 2016-06-01-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
publicationNumber | CN-105622329-A |
titleOfInvention | Synthetic method for flurazepam drug intermediate o-fluorotoluene |
abstract | The invention discloses a synthetic method for a flurazepam drug intermediate o-fluorotoluene. The method comprises the following steps: (i) in a reaction container equipped with a stirrer, a temperature meter and a drop funnel, adding 200-230ml of a strong phosphoric acid solution, cooling the solution to 15-20 DEG C, adding 1.2mol of o-toluidine, after o-toluidine is completely dissolved, cooling the solution to 5-9 DEG C, adding 1.2-1.25mol of potassium nitrite to be dissolved in the solution, controlling the reaction temperature to be 5-8 DEG C, measuring a reaction termination point by using potassium iodide test paper, and obtaining diazonium salt; and (ii) cooling 1.4mol of a sodium fluoride solution to 3-5 DEG C, adding a diazonium salt solution generated in the step (i), stirring for 6-9 minutes, performing suction filtration, washing a filter cake with a phosphoric acid solution, a washing solvent and a neutral solution in sequence, drying in vacuum to obtain fluorine-containing diazonium salt (3), heating the fluorine-containing diazonium salt to 90-98 DEG C for decomposing the fluorine-containing diazonium salt, collecting distillate, washing the distillate with a potassium carbonate solution and a salt solution in sequence, drying by a dehydrating agent, performing low-pressure distillation, and collecting cut fraction with the temperature of 103-110 DEG C to obtain a colorless liquid o-fluorotoluene. |
isCitedBy | http://rdf.ncbi.nlm.nih.gov/pubchem/patent/CN-106336340-B http://rdf.ncbi.nlm.nih.gov/pubchem/patent/CN-106336340-A |
priorityDate | 2015-12-23-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
type | http://data.epo.org/linked-data/def/patent/Publication |
Incoming Links
Total number of triples: 45.