(CH3)2NSFAsF–Synthesis and Stability of a Simple Pentacoordinated Sulfur(VI) Cation

✍ Scribed by Dipl.-Chem. Thomas Meier; Prof. Dr. Rüdiger Mews

• Book ID: 101556930
• Publisher: John Wiley and Sons
• Year: 1985
• Tongue: English
• Weight: 211 KB
• Volume: 24
• Category: Article
• ISSN: 0044-8249
• DOI: 10.1002/anie.198503441

✦ Synopsis

gradation that occurs through cleavage of ether and C-C bondst3] in the potassium reduction cannot be quantified. We are therefore attempting to attach alkanesulfonic acid groups to the coal skeleton via non-reductive reactions.

Experimental procedure

Finely ground coal (I0 g, average particle diameter 60 pm) was stirred at -25°C for 24 h in a "blue solution", which had been prepared by adding potassium (10 g, 256 mmol) in small pieces to 300 mL of dimethoxyethane and 50 mL of polyethylene glycol dimethyl ether ("octaglyme")."' After unreacted potassium (ca. 3.4 g) had been removed I (31.2 g, 256 mmol), dissolved in 20 mL of dimethoxyethane, was added within 10 min and the mixture was then stirred for 24 h at -25°C. After the solvent had been distilled off, the residue was extracted with ether in a Soxhlet apparatus for 3 d and dried. All water-soluble reagents were removed by suspending the material in 200 mL of hydrochloric acid (50% v/v) and centrifuging in order to isolate the product; this process was carried out six times. The residue, after washing once more on a glass filter with acetone and drying (3 d at lo-' torr and 25"C), yielded 13.1 g dark 2.I9l