Cobalt Pentazolate was Synthesized in Complete One Pot
In order to synthesize cobalt pentazolate conveniently,using 2,6-dimethyl-4-aminophenol hydrochloride as the raw material,the diazotization/cyclization/C—N cleavage"complete one-pot"synthesis reaction,condition exploration,separation and purification were studied.Cobalt pentazolate was characterized by infrared(IR),ion chromatography(IC)and X-ray single crystal diffraction.The results showed that cobalt pentazolate can be easily synthesized via the diazotization/cyclization/C—N cleavage"complete one-pot"method.The optimum conditions were as follows:methanol as diazoti-zation solvent,tetrafluoroboric acid/isoamyl nitrite as diazotization reagent,sodium azide was added in solid form,cyclization reaction time is 16 h,cobalt pentazolate can be easily obtained by direct precip-itation method.Ion chromatography(IC)showed that the purity of cobalt pentazolate was up to 98.93%(area normalization).This method avoids complicated experimental operation and possible safety problems,and provides a new idea and direction for the synthesis and process amplification of pentazolate compounds.