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DOI: 10.3791/57455-v
Here, we present a one-pot, transition-metal-free synthesis of thiols and thioesters from aromatic halides and sodium thiomethoxide, followed by the preparation of single crystals of a metal-dithiolene network using thiol species generated in situ from the more stable and tractable thioester.
The overall goal of this protocol is to synthesize thiol linker molecules and to prepare single crystals of porous, metal-sulfur frameworks from these thiol species. This method can help answer key questions in the field of materials chemistry as to how to better prepare crystalline networks from metal ions and mercaptan molecules. The main advantage of this technique is provided by the convenient and reduced-time synthesis which utilize the relative stable thioester as the precursor for framework assembly.
Demonstrating the procedure will be Mr.He Yonghe, a graduate student in my laboratory. To begin the procedure, connect a 200 milliliter Schlenk flask, equipped with a stir bar, to a vacuum-gas manifold. Evacuate and backfill the flask with nitrogen gas three times.
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