Topics in Current Chemistry

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Topics in Current Chemistry ( topics-current-chemistry )

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Solid Sulfur Allotropes 13 Scheme 1 2.1.1.12 Preparation of S18 1. Preparation of S18 from S2Cl2 and potassium iodide: dichlorodisulfane, dis- solved in CS2, reacts at 20 􏰹C with aqueous potassium iodide to a mixture of even-membered sulfur rings; see Eq. (21). The main product is S6 (36%; see above) but by a sequence of precipitation and extraction procedures S12 (1– 2%), endo-S18 (0.4%), and S20 (0.4%) have been prepared in pure form in the yields given in parentheses [11]. 2. From liquid sulfur: small amounts of endo-S18 have been isolated from quenched sulfur melts by extraction and fractional crystallization; see above under “Preparation of S12, S18, and S20 from liquid sulfur”. 2.1.1.13 Preparation of S20 cyclo-Eicosasulfur S20 has been prepared by different methods. Most conve- nient is the synthesis by sulfur transfer from titanocene pentasulfide which, depending on the conditions, provides either S10, S15 or S20. 1. By ligand transfer: a procedure optimized for the preparation of S20 uses the reaction of sulfurylchloride with titanocene pentasulfide in CS2 at 25 􏰹:

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