Sulfur Dioxide → Sulfur Dioxide

A solution of sulfur dioxide was prepared by bubbling sulfur dioxide (3.9 g, 61 mmol) in a solution of anhydrous acetonitrile (20 ml) at ambient temperature. This solution was added to PhSCF2SiMe3 (4.3 g, 18.4 mmol, obtained according to the procedure from example 6) and stirred at ambient temperature under an inert atmosphere. Anhydrous CsF (2.8 g, 18.5 mmol) was then added to the reaction mixture, which was stirred at ambient temperature overnight. The reaction was monitored by TLC and by 19F NMR (CDCl3) until the disappearance of PhSCF2SiMe3. F-TEDA (7.15 g, 20 mmol) was added to the mixture, at −20° C., which was then stirred for 1 h at ambient temperature. The mixture was concentrated and the solid residue washed with ethyl ether (10×50 ml). The filtrate was evaporated and the product purified by bulb-to-bulb distillation. The product difluoro(phenylsulfanyl)methanesulfonyl fluoride was obtained in the form of a colorless liquid (2.5 g, 57%).

1. customobtained
2. stirringwas stirred at ambient temperature overnight
3. stirringwhich was then stirred for 1 h at ambient temperature
4. concentrationThe mixture was concentrated
5. washthe solid residue washed with ethyl ether (10×50 ml)
6. customThe filtrate was evaporated
7. distillationthe product purified by bulb-to-bulb distillation

ORDレコード

ord-4fd926c4374d4e32a57a352e63167b10

出典データセット

uspto-grants-2014_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08853448B2