fluorosulfonyloxyethane

Conditions: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: Five g of 7-methoxybenzotelluropyrone was added to 20 ml of freshly distilled ethyl fluorosulfonate. The resulting mixture was stirred under nitrogen at 60° C. for 10 minutes. Two hundred ml of ether was added precipitating a red solid. The product was collected by filtration and recrystallized from acetonitrile to give 6.0 g (87%) of a red solid. precipitating a red solid The product was collected by filtration recrystallized from acetonitrile

Conditions: temp:25.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A solution of 9.2 g (0.09 mol) of triethylamine in 25 ml of ether was added dropwise to a stirred solution of 17.6 g (0.10 mol) of trifluoromethylmalonyl fluoride in 50 ml of ether at -80°C. To the resulting suspension of solid was added 14.1 g (0.11 mol) of ethyl fluorosulfate and the mixture was then allowed to warm to 25°C with stirring. The homogeneous reaction mixture developed two layers after standing overnight. Distillation gave 15 g (74%) of ethyltrifluoromethylmalonyl fluoride, bp 54°-56°C (260 mm), identified by ir. To the resulting suspension of solid Distillation