完全一锅法合成五唑钴
Cobalt Pentazolate was Synthesized in Complete One Pot
李金勇 1张思宇 1龙婷 1黄明 2罗郑航 1杨海君1
作者信息
- 1. 西南科技大学材料与化学学院,四川绵阳 621010
- 2. 中国工程物理研究院化工材料研究所,四川绵阳 621999
- 折叠
摘要
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.
Abstract
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.
关键词
完全一锅法/合成条件/表征/五唑钴/单晶Key words
complete one-pot/synthesis condition/characterization/pentazolate cobalt/single crystal引用本文复制引用
基金项目
国家自然科学基金面上项目(22075260)
四川省自然科学基金面上项目(2022NSFSC0288)
出版年
2024
NETL
NSTL
维普
万方数据