http://rdf.ncbi.nlm.nih.gov/pubchem/patent/CN-106431964-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/C07C247-16 |
classificationIPCInventive | http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07C247-16 |
filingDate | 2016-09-19-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
inventor | http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_a29b69639283e74eb7b72639403b7745 |
publicationDate | 2017-02-22-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
publicationNumber | CN-106431964-A |
titleOfInvention | Synthesis method of azaguanine drug intermediate azidobenzene |
abstract | A synthesis method of an azaguanine drug intermediate azidobenzene comprises steps as follows: 0.32 mol of stannous chloride and 310 ml of a potassium bromide solution are added to a reaction container, the temperature of the solution is reduced to 5-8 DEG C, the stirring speed is controlled to be 130-160 rpm, 0.36 mol of phenylhydrazine is added, the dropwise adding time is controlled in 30-50 min, white precipitates are separated out from the solution, the temperature of the solution is reduced to 2-4 DEG C, 300 ml of cyclohexanone is added, 0.41-0.43 mol of o-nitrotoluene is dropwise added, the dropwise adding time is controlled in 60-80 min, atmospheric distillation is performed, a water layer is separated out from distillate, cyclohexanone is used for extraction, cyclohexanone layers are mixed, dehydration is performed with a dehydrating agent, filtration is performed, washing is performed with a salt solution and ethanediamine sequentially, reduced pressure distillation is performed after cyclohexanone is recovered, fractions at the temperature of 80-85 DEG C are collected, recrystallization is performed in ethyl acetate, and azidobenzene crystals are obtained. |
priorityDate | 2015-12-25-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
type | http://data.epo.org/linked-data/def/patent/Publication |
Incoming Links
Total number of triples: 64.