http://rdf.ncbi.nlm.nih.gov/pubchem/patent/CN-106397278-A
Outgoing Links
Predicate | Object |
---|---|
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 |
Incoming Links
Total number of triples: 36.