3,3,3-trifluoro-2-(trifluoromethyl)propanoyl fluoride

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

Procedure: The above methyl ether, 48.5 g (0.209 mol), and 1 g of AlCl3 were refluxed together for 15 hours and treated as described in Comparative Example 1. An amount of 43.8 g of unreacted (CF3)2CHCF2OCH3 was recovered, together with 1.1 g of (CF3)2CHCOF (2.7% yield) and 0.75 g of CH3F. No improvement in product was obtained when the reactants were heated in a sealed tube at 120° for 4 hours. treated

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

Procedure: The above ethyl ether, 43 g (0.175 mol), in a 100 ml flask equipped as described in Example 6 was mixed with 1 g (0.0075 mol) of AlCl3. The mixture was refluxed for 17 hours. Material condensed in the attached Dry Ice-acetone trap was combined with residual material in the flask and distilled in a low-temperature still. An amount of 30.8 g of unreacted (CF3)2CHCF2OC2H5 was recovered, together with 9.1 g (26.3% yield) of (CF3)2CHCOF, 2.2 g of C2H5F and 0.1 g of (CF3)2CHCOCl. No improvement in product yield was obtained when the reactants were heated in a sealed tube at 120° for 4 hours. The mixture was refluxed for 17 hours Material condensed in the distilled in a low-temperature still