http://rdf.ncbi.nlm.nih.gov/pubchem/patent/CN-106431955-A

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assignee http://rdf.ncbi.nlm.nih.gov/pubchem/patentassignee/MD5_17fa04088f285d891117ee10818886c0
classificationCPCInventive http://rdf.ncbi.nlm.nih.gov/pubchem/patentcpc/C07C231-08
classificationIPCInventive http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07C231-08
http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07C233-07
filingDate 2016-09-18-04:00^^<http://www.w3.org/2001/XMLSchema#date>
inventor http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_9396db198628b4c20cec9bb4939183de
publicationDate 2017-02-22-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationNumber CN-106431955-A
titleOfInvention Synthesis method of tocainide drug intermediate alpha-bromopropionyl-2,6-dimethylaniline
abstract The invention discloses a synthesis method of a tocainide drug intermediate alpha-bromopropionyl-2,6-dimethylaniline. The synthesis method comprises the following steps of (i) adding 1.55mol of 2,6-dimethylaniline and 2.4L to 2.6L of isopropanol into a reactor vessel provided with an agitator, a thermometer, a reflux condenser and a dropping funnel, controlling an agitation speed to be 130rpm to 150rpm, heating a solution until a temperature is 85 to 90 DEG C, maintaining the temperature for 30min to 40min, decreasing the temperature of the solution to 40 to 45 DEG C, dropwise adding 1.89mol to 1.91mol of alpha-bromopropanamide, refluxing and making an obtained mixture react for 9h to 10h after the addition is finished, decreasing the temperature of the solution to 3 to 6 DEG C, making the solution stand for 28h to 32h, filtering the solution, separating out a solid, washing the solid by using an ether solution, then washing the solid by using a saline solution, dehydrating the solid with a dehydrating agent, and then recrystallizing the solid by using a triethylamine solution, so as to obtain the alpha-bromopropionyl-2,6-dimethylaniline, wherein the mass fraction of the isopropanol in the step (1) is 85 to 90 percent, and the mass fraction of the ether solution in the step (1) is 90 to 95 percent.
priorityDate 2015-12-22-04:00^^<http://www.w3.org/2001/XMLSchema#date>
type http://data.epo.org/linked-data/def/patent/Publication

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