[CH2:1](N(CC)CC)[CH3:2].[F:8][C:9]([CH:12]([C:16]([F:18])=[O:17])[C:13]([F:15])=[O:14])([F:11])[F:10].S(F)(OCC)(=O)=O>CCOCC>[CH2:1]([C:12]([C:9]([F:11])([F:10])[F:8])([C:13]([F:15])=[O:14])[C:16]([F:18])=[O:17])[CH3:2]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.
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