http://rdf.ncbi.nlm.nih.gov/pubchem/patent/EP-1162198-A1

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filingDate 2001-06-05-04:00^^<http://www.w3.org/2001/XMLSchema#date>
inventor http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_686d420f5705b85e055166270d896da5
http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_0b944018cb3152459e59c39f6abb4f7a
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publicationDate 2001-12-12-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationNumber EP-1162198-A1
titleOfInvention Process for the preparation of highly pure 5,5'-bi-1H tetrazolediammonium salts
abstract A process for the preparation of a highly pure 5,5'-bi-1H-tetrazolediammoniumnsalt (BHT·2NH 3 ) in a high yieldnby efficiently synthesizing the 5,5'-bi-1H-tetrazolediammoniumnsalt (BHT·2NH 3 ) from cheap and easy-to-handlenstarting materials based on a one-pot reaction,nand removing copper components which are impurities in thenform of a copper·ammonia·5,5'-bi-1H-tetrazole complex fromnthe reaction solution or from the coarse crystals isolatednfrom the reaction solution. By further conducting thentreatment with a chelating resin, the copper content cannbe further decreased. n The refining process is conducted by either:n (A) adding small amounts of aqueous hydrogen peroxide andnammonia water to the reaction solution containing then5,5'-bi-1H-tetrazoledisodium salt that is obtained bynsynthesizing a dicyan by adding, as an oxidizing agent, anaqueous hydrogen peroxide to an aqueous solution of thenstarting materials of which the pH has been adjusted to ben5 to 7 by the addition of a small amount of acidicnsubstance in the presence of hydrogen cyanide or sodiumncyanide, sodium azide and a catalytic amount of a coppernsalt, followed by the heat-cyclization reaction, andnremoving by filtration the insoluble component of thenprecipitated copper·ammonia·5,5'-bi-1H-tetrazole complex,nand reacting the reaction solution with an aqueousnsolution of ammonium chloride, or (B) adding the aqueous solution of ammonium chloride tonthe reaction solution, transforming the separated 5,5'-bi-1H-tetrazolediammoniumnsalt (BHT·2NH 3 ) into a 5,5'-bi-1H-tetrazoledisodiumnsalt (BHT·2Na), dissolving the disodiumnsalt again, and reacting the aqueous solution of thenobtained 5,5'-bi-1H-tetrazoledisodium salt from which theninsoluble component of the formed copper·ammonia·5,5'-bi-1H-tetrazole ncomplex has been removed by filtration withnthe aqueous solution of ammonium chloride. The process ofnpreparing the highly pure 5,5'-bi-1H-tetrazolediammoniumnsalt (BHT·2NH 3 ) combines the refining process (A) or (B)nwith a step of treatment with a chelating resin to reactnthe treated solution with ammonium chloride or an aqueousnsolution thereof to recover the formed highly purenammonium salt in the form of crystals.
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