http://rdf.ncbi.nlm.nih.gov/pubchem/patent/CN-105503491-A

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assignee http://rdf.ncbi.nlm.nih.gov/pubchem/patentassignee/MD5_55d2d8989f1d88678e523954a877413e
classificationCPCInventive http://rdf.ncbi.nlm.nih.gov/pubchem/patentcpc/C07C1-00
classificationIPCInventive http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07C11-22
http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07C1-00
filingDate 2015-12-25-04:00^^<http://www.w3.org/2001/XMLSchema#date>
inventor http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_e6d7cc0afcf466d528626c61da3bc04b
publicationDate 2016-04-20-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationNumber CN-105503491-A
titleOfInvention Synthesis method of terbinafine medical intermediate tert-butyl acetylene
abstract A synthesis method of terbinafine medical intermediate tert-butyl acetylene includes the following steps of adding 310 ml of potassium bisulfite solution and 300 ml of potassium bisulfite to a reaction vessel provided with a stirrer, a thermometer, a dropping funnel and a condenser, raising the temperature of the solution to 90-95 DEG C, controlling the stirring speed at 150-170 rpm, dropwise adding 0.73 mol of 1,1-diamido-3,3-dimethylbutane, controlling the dropwise adding time at 3-5 hours, adding 0.81-0.84 mol of hypochloric acid phenyl ester, conducting reaction for 90-120 min, raising the temperature of the solution to 110-115 DEG C, continuing to conduct reaction for 3-5 hours, lowering the temperature of the solution to 10-15 DEG C, separating out solid, conducting filtering, saline solution washing, acetonitrile washing and pressure reduction distillation, collecting fraction of 100-108 DEG C, and conducting recrystallization in cyclohexane to obtain crystal tert-butyl acetylene.
priorityDate 2015-12-25-04:00^^<http://www.w3.org/2001/XMLSchema#date>
type http://data.epo.org/linked-data/def/patent/Publication

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