http://rdf.ncbi.nlm.nih.gov/pubchem/patent/CN-106431992-A

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Predicate Object
assignee http://rdf.ncbi.nlm.nih.gov/pubchem/patentassignee/MD5_17fa04088f285d891117ee10818886c0
classificationCPCInventive http://rdf.ncbi.nlm.nih.gov/pubchem/patentcpc/C07C269-08
http://rdf.ncbi.nlm.nih.gov/pubchem/patentcpc/C07C269-04
classificationIPCInventive http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07C271-22
http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07C269-08
http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07C269-04
filingDate 2016-09-18^^<http://www.w3.org/2001/XMLSchema#date>
inventor http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_9396db198628b4c20cec9bb4939183de
publicationDate 2017-02-22^^<http://www.w3.org/2001/XMLSchema#date>
publicationNumber CN-106431992-A
titleOfInvention Synthesis method of hydroxylamine imidazole cephalosporin propylene glycol drug intermediate D-alpha-tert-butoxy carbonyl amino-alpha-(4-hydroxyphenyl)-acetic acid
abstract The invention discloses a synthesis method of a hydroxylamine imidazole cephalosporin propylene glycol drug intermediate D-alpha-tert-butoxy carbonyl amino-alpha-(4-hydroxyphenyl)-acetic acid. The method comprises the following steps: (i), adding 200 ml of a propionitrile solution, 0.06 mol of D-(-)-hydroxy phenylglycine and 0.08 mol of sodium bromide into a reactor provided with a stirrer, a condensation backflow device and a thermometer, controlling a stirring speed to range from 160 rpm to 190 rpm, controlling stirring time to range from 90 min to 120 min, adding 0.081-0.085 mol of tert-butoxycarbonylation bromine slowly in batches, controlling solution temperature to range from 60 DEG C to 65 DEG C, controlling reaction time to range from 19 h to 20 h, adding 500 ml of a potassium bromide solution for dilution, performing ethidene diamine extraction for 6-8 times, washing a water layer with oxalic acid, controlling solution pH to range from 5 to 6, performing ethidene diamine extraction for 4-5 times after adding potassium bromide to be saturated, dehydrating an extract with calcium chloride, performing pressure reduction distillation to steam a solvent out, adding residues into a butanol solution, and smashing and filtering a solid to obtain the D-alpha-tert-butoxy carbonyl amino-alpha-(4-hydroxyphenyl)-acetic acid, wherein the mass fraction of the propionitrile solution in the step (i) is 55-65%, and the mass fraction of the potassium bromide solution in the step (i) is 35-40%.
priorityDate 2015-12-22^^<http://www.w3.org/2001/XMLSchema#date>
type http://data.epo.org/linked-data/def/patent/Publication

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