http://rdf.ncbi.nlm.nih.gov/pubchem/patent/CN-106397278-A

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assignee http://rdf.ncbi.nlm.nih.gov/pubchem/patentassignee/MD5_44b2f7427db73e272b2ca198cea89dcd
classificationCPCInventive http://rdf.ncbi.nlm.nih.gov/pubchem/patentcpc/C07C303-28
classificationIPCInventive http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07C309-66
http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07C303-28
filingDate 2016-09-11-04:00^^<http://www.w3.org/2001/XMLSchema#date>
inventor http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_4d26be540194e25398279f51879c1a9d
publicationDate 2017-02-15-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationNumber CN-106397278-A
titleOfInvention Synthesis method for busulphan medicament intermediate 1,4-di-methanesulfonic butane diester
abstract The invention discloses a synthesis method for busulphan medicament intermediate 1,4-di-methanesulfonic butane diester. The synthesis method comprises the following steps: adding 0.15mol of 1,4-butanediol and 150-170ml of triethylamine into a reaction vessel, and reducing the temperature of a solution to 3-5 DEG C; controlling the stirring speed to be 130-160 rpm, and slowly dropwise adding 0.36-0.38 mol of ammonium methanesulfonate; after dropwise adding, increasing the temperature of the solution to 35-40 DEG C, stirring for 3-4h, and reducing the temperature of solution to 15-20 DEG C so as to separate out a solid; performing filtration, washing with a saline solution, performing dehydration by use of a dehydrator, and recrystallizing in cyclohexane, thereby obtaining a white solid, namely 1,4-di-methanesulfonic butane diester, wherein the saline solution adopted in the step is any one of sodium nitrate and potassium sulfate.
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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