http://rdf.ncbi.nlm.nih.gov/pubchem/patent/CN-105461631-A

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assignee http://rdf.ncbi.nlm.nih.gov/pubchem/patentassignee/MD5_122bbcbc574a179c8e4e5eb17c0dae56
classificationCPCInventive http://rdf.ncbi.nlm.nih.gov/pubchem/patentcpc/C07D233-64
classificationIPCInventive http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07D233-64
filingDate 2015-12-24-04:00^^<http://www.w3.org/2001/XMLSchema#date>
inventor http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_8945730e366d5f6b5a4db4547d4e2572
publicationDate 2016-04-06-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationNumber CN-105461631-A
titleOfInvention Synthetic method of methimidol hydrochloride medicine intermediate 1-(beta-hydroxyethyl)-2-methylimidazole
abstract The present invention relates to a synthetic method of a methimidol hydrochloride medicine intermediate 1-(beta- hydroxyethyl)-2-methylimidazole. The synthetic method comprises the following steps: adding 1.3 mol of 2-methylimidazole (2), 1.5 to 1.7 mol of ethamine alcohol and 200 ml of nitroethane into a reaction vessel with a stirrer, a thermometer and a reflux condenser, increasing the temperature of a solution to 70 to 75 DEG C, refluxing for 9 to 10 h, lowering the temperature of the solution to 50 to 55 DEG C, standing and layering, taking out lower liquid, dissolving in 1.3 to 1.6 L of propionitrile, lowering the temperature of the solution to 13 to 15 DEG C, adding 130 ml of oxalic acid, lowering the temperature of the solution to 2 to 4 DEG C, suction filtering, washing by using 130 ml of cyclohexane, re-crystallizing in acetonitrile, decoloring by virtue of a molecular sieve, controlling a stirring speed at 90 to 110 rpm, precipitating solids 2 to 3 h later, washing by virtue of a saline solution, washing by virtue of isopropanol, dedydrating by virtue of a dehydrating agent, and drying at 70 to 75 DEG C to obtain 1-(beta-hydroxyethyl)-2-methylimidazole, wherein the mass percent of the propionitrile in the step is 80 to 85 percent, the mass percent of the oxalic acid in the step is 30 to 35 percent, and the mass percent of cyclohexane in the step is 70 to 75 percent.
isCitedBy http://rdf.ncbi.nlm.nih.gov/pubchem/patent/CN-112851694-A
priorityDate 2015-12-24-04:00^^<http://www.w3.org/2001/XMLSchema#date>
type http://data.epo.org/linked-data/def/patent/Publication

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