Preparation and purification of zinc sulfinate reagents for drug discovery.
Preparation and purification of zinc sulfinate reagents for drug discovery.
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DOI：
10.1038/nprot.2013.059
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发表时间：
2013-06
期刊：
影响因子：
14.8
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中科院分区：
文献类型：
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本协议详细介绍了双（链烷亚磺酸）锌的合成，该锌可用作自由基物质形成的通用试剂。本文所述的亚磺酸锌是通过用锌粉处理由相应的磺酰氯产生的。产物可以粗制使用，或者可以进行简单的纯化程序以最小化水和氯化锌的掺入。进行了元素分析以确认亚磺酸锌试剂的纯度；还进行了与咖啡因的反应，以验证已合成的每批产品的反应性。虽然亚磺酸锌盐的合成通常在 3 小时内进行，但后处理可能需要长达 24 小时，纯化可能需要长达 3 小时。遵循本协议中的步骤将使用户能够在一周内生成亚磺酸锌试剂的小型工具包。
The present protocol details the synthesis of zinc bis(alkanesulphinate)s that can be used as general reagents for the formation of radical species. The zinc sulphinates described herein have been generated from the corresponding sulphonyl chlorides by treatment with zinc dust. The products may be used crude, or a simple purification procedure may be performed to minimize incorporation of water and zinc chloride. Elemental analysis has been conducted in order to confirm the purity of the zinc sulphinate reagents; reactions with caffeine have also been carried out to verify the reactivity of each batch that has been synthesized. Although the synthesis of the zinc sulphinate salts generally proceeds within 3 h, workup can take up to 24 h and purification can take up to 3 h. Following the steps in this protocol would enable the user to generate a small toolkit of zinc sulphinate reagents over the course of one week.