Thionyl Chloride → 2-Chloro-2,3,3-trifluoro-1-methylcyclobutane-1-carbonyl chloride

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Reaction Steps

One drop of dimethylformamide is added to a mixture of 91.2 g (0.45 mol) of 1-methyl-2,3,3-trifluoro-2-chlorocyclobutane-1-carboxylic acid and 450 ml of chloroform. After this, 80.3 g (0.675 mol) of thionyl chloride are added dropwise at 25°-30° C. with stirring, and the stirred mixture is heated to the boil. After 6 hours the mixture is cooled, the solvent is stripped off, and the residue is subjected to fractional distillation under reduced pressure. 75 g (75% of theory) of 1-methyl-2-chloro-2,3,3-trifluoro-cyclobutane-1-carbonyl chloride are obtained in form of a liquid of boiling point 65°-70° C. at 20 mbar. ##STR60##

Provenance & Evidence