http://rdf.ncbi.nlm.nih.gov/pubchem/patent/CN-105481804-A

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assignee http://rdf.ncbi.nlm.nih.gov/pubchem/patentassignee/MD5_55d2d8989f1d88678e523954a877413e
classificationCPCAdditional http://rdf.ncbi.nlm.nih.gov/pubchem/patentcpc/C07B2200-13
classificationCPCInventive http://rdf.ncbi.nlm.nih.gov/pubchem/patentcpc/C07D307-52
classificationIPCInventive http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07D307-52
filingDate 2015-12-25-04:00^^<http://www.w3.org/2001/XMLSchema#date>
inventor http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_c7d837e2e2d85953e8da70ceb9a24166
publicationDate 2016-04-13-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationNumber CN-105481804-A
titleOfInvention Synthesis method of furtrethonium iodide drug intermediate 2-dimethylaminomethylfuran
abstract The invention relates to a synthesis method of a furtrethonium iodide drug intermediate 2-dimethylaminomethylfuran, which comprises the following steps: adding 1.6 mol of dimethylcarbinol amine solution, 500ml of oxalic acid solution, 1.8 mol of aluminum oxide and 2.1-2.6 mol of 2-furyldimethyl alcohol solution into a reaction vessel which is provided with a stirrer, a thermometer and a dropping funnel, controlling the stirring rate at 130-170 rpm, heating the solution to 120-128 DEG C, reacting for 5-8 hours, cooling the solution to 90-96 DEG C, refluxing for 2-3 hours, cooling, adding 130ml of phosphoric acid solution, heating the solution to 60-66 DEG C, stirring to react for 90-130 minutes, adding 300ml of sodium sulfite solution, continuing reacting for 80-110 minutes, cooling the solution to 10-15 DEG C, adding 110ml of potassium bisulfite solution, standing for 3-5 hours to stratify the solution, separating out the oil layer, extracting the water layer with nitromethane 5-8 times, merging the oil layers, dehydrating with dehydrating agent, carrying out reduced pressure distillation, collecting the 110-116-DEG C fraction, and recrystallizing in toluene to obtain the crystal 2-dimethylaminomethylfuran.
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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