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Purification of Laboratory Chemicals, 8th Edition by W.L.F. Armarego

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Bis(trimethylsilyl) sulfide (hexamethyldisilathiane) [3385-94-2] C6H18SSi2, M 178.5, b 65-67°/16mm, 162.5-163.5°/750mm, 164°/760mm, d420 0.85, nD20 1.4598. Dissolve it in petroleum ether (b ca 40°), remove the solvent and distil it. Redistil it under atmospheric pressure of dry N2. It is collected as a colourless liquid which solidifies to a white solid in Dry-ice. On standing for several days it turns yellow possibly due to liberation of sulfur. Store it below 4° under dry N2. It is prepared by adding Ag2S (37g, 0.15mol) to Me3SiI (40g, 0.2mol, see 16029-98-4 below) and heating under reflux for 14 hours when the temperature rises to 150°. Distil off the liquid from the solid and redistil to give the disilathiane (13g, 73%). The boiling time ...

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