http://rdf.ncbi.nlm.nih.gov/pubchem/patent/CN-105461631-A
Outgoing Links
Predicate | Object |
---|---|
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 |
Incoming Links
Total number of triples: 60.