Syntheses and Reactions of 2,5‐Disulfobenzene‐1‐diazonium Salts: Towards Functionalized Sulfonate Metal–Organic Frameworks
Syntheses and Reactions of 2,5‐Disulfobenzene‐1‐diazonium Salts: Towards Functionalized Sulfonate Metal–Organic Frameworks
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DOI：
10.1002/ejoc.201001436
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发表时间：
2011-03
影响因子：
2.8
通讯作者：
Thomas W. T. Muesmann;J. Ohlert;M. Wickleder;J. Christoffers
中科院分区：
文献类型：
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作者：
Thomas W. T. Muesmann;J. Ohlert;M. Wickleder;J. Christoffers
研究了钡盐结晶及阳离子交换树脂质子化制备2-取代1，4-苯二磺酸的方法。该技术应用于2-氯-、2-溴-、2-碘-和2-羟基-1，4-苯二磺酸的制备。使碘代衍生物进行以Pd/C作为催化剂的Suzuki偶联反应，随后分离相应的联苯衍生物。制备碘二磺酸的铜（II）盐。在固态下，发现形成聚合物链，其在二维层中互锁。发现该材料在高达400 °C的温度下是热稳定的，高于该温度，盐分解得到CuI。
A preparation, separation, and purification protocol for 2-substituted 1,4-benzenedisulfonic acids by exploiting crystallization of the barium salts and their subsequent protonation with cation-exchange resin was developed. This technique was applied to the preparation of 2-chloro-, 2-bromo-, 2-iodo-, and 2-hydroxy-1,4-benzenedisulfonic acids. The iodo derivative was submitted to Suzuki coupling reactions with Pd/C as the catalyst, and the respective biphenyl derivatives were subsequently isolated. The copper(II) salt of the iododisulfonic acid was prepared. In the solid state, it was found to form polymeric chains, which interlock in two-dimensional layers. The material was found to be thermally stable up to 400 °C above which point the salt decomposed to afford CuI.