文献类型：期刊文献

中文题名：5-氮螺[4.4]壬烷四氟硼酸盐的新合成方法

英文题名：New synthetic method of 5-azoniaspiro[4.4]nonane tetrafluoroborate

作者：冯磊[1];闫薪竹[1];朱鹏飞[1];施苏萍[2];关士友[1]

机构：[1]华东理工大学材料科学与工程学院,上海200237;[2]江苏国泰超威新材料有限公司,苏州215634

年份：2015

卷号：43

期号：9

起止页码：45

中文期刊名：化工新型材料

外文期刊名：New Chemical Materials

收录：北大核心:【北大核心2014】；CSCD:【CSCD2015_2016】；

基金：国家自然科学基金资助项目(20973060)

语种：中文

中文关键词：5-氮鎓螺[4.4]壬烷四氟硼酸盐;SBP-BF4;合成;亲核;反应;钾;钠

外文关键词：5-azoniaspiro [4.4] nonane tetrafluoroborate, SBP-BF4, synthesis, nucleophile, reaction, potassium,sodium

摘要：利用氨与1,4-二碘丁烷的亲核反应,得到5-氮螺[4.4]壬烷碘盐(SBP-I),再通过SBP-I与四氟硼酸的离子交换反应,制得5-氮螺[4.4]壬烷四氟硼酸盐(SBP-BF4)。采用核磁、离子色谱和等离子发射光谱对合成产物进行了表征。通过单因素法考察了反应温度、反应时间对SBP-I产率的影响,结果表明:在反应温度为50℃,反应时间为24h条件下,SBP-I产率可达87%;最终产物中,钾、钠等金属离子总质量分数小于1.2×10-5。与传统方法相比,该合成法不仅降低了原料成本,还可有效避免引入金属离子杂质。
5-azoniaspiro[4.4]nonane iodide （SBP-I） was prepared by nucleophilic reaction of ammonia with 1,4-diiodobutane, then 5-azoniaspiro[4.4] nonane tetrafluoroborate salt was prepared by ion exchange of between SBP-I and tetrafluoroboric acid. The products were characterized by ^1H-NMR, ion chromatography and plasma emission spectroscopy. The influence of reaction temperature and reaction time on the SBP-I yield were studied by single factor, the results showed that：when the reaction temperature was 50℃, reaction time was 24h, the yield of SBP I was up to 87%,and the total content of potassium, sodium and other metals plasma was less than 12ppm in the final product. Compared with traditional methods,this method not only reduced the cost of raw materials but also effectively avoided the introduction of metal ion impurities.