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完全一锅法合成五唑钴

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为了简便合成五唑钴,以2,6-二甲基-4-氨基苯酚盐酸盐为原料,开展了重氮化/环化/C—N键切断"完全一锅法"的合成反应、条件探索及分离纯化研究.通过红外(IR)、离子色谱(IC)、X-射线单晶衍射等方法对五唑钴进行了分析表征.结果表明:重氮化/环化/C—N键切断"完全一锅法"可以简便地合成得到五唑钴.适宜条件为:以甲醇为重氮化溶剂,四氟硼酸/亚硝酸异戊酯作为重氮化试剂,叠氮化钠以固体形式加入,环化反应时间为16 h,经直接沉淀法即可简便地得到五唑钴.离子色谱表明:所合成的五唑钴纯度高达98.93%(面积归一法).该方法避免了繁琐的实验操作和可能引发的安全问题,为五唑化合物的合成和工艺放大提供新的思路和方向.
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.

complete one-potsynthesis conditioncharacterizationpentazolate cobaltsingle crystal

李金勇、张思宇、龙婷、黄明、罗郑航、杨海君

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西南科技大学材料与化学学院,四川绵阳 621010

中国工程物理研究院化工材料研究所,四川绵阳 621999

完全一锅法 合成条件 表征 五唑钴 单晶

国家自然科学基金面上项目四川省自然科学基金面上项目

220752602022NSFSC0288

2024

合成化学
四川省化学化工学会 中国科学院成都有机化学研究所

合成化学

CSTPCD
影响因子:0.42
ISSN:1005-1511
年,卷(期):2024.32(1)
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