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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。
The nucleophilic reaction of ammonia with 1, 4-diiodobutane gives 5-azaspiro [4.4] nonane iodonium salt (SBP-I), followed by ion exchange reaction with SBP-I and tetrafluoroboric acid 5-Azaspiro [4.4] nonane tetrafluoroborate (SBP-BF4). The synthesized products were characterized by NMR, ion chromatography and plasma emission spectroscopy. The effects of reaction temperature and reaction time on the yield of SBP-I were investigated by single factor method. The results showed that the yield of SBP-I reached 87% at 50 ℃ for 24 h. The final product , Potassium, sodium and other metal ions total mass fraction of less than 1.2 × 10-5. Compared with the traditional method, the synthesis method not only reduces the cost of raw materials, but also can effectively avoid the introduction of metal ion impurities.