反应详情

19.4 g (0.058 mol) of 2,2-dimethyl-3-(2-chloro-2-(4-trifluoromethoxy-phenyl)-vinyl)-cyclopropanecarboxylic acid were dissolved in 150 ml of carbon tetrachloride, and 15 g of thionyl chloride were slowly added dropwise at 25° C., while stirring. The mixture was then heated to the reflux temperature for 4 hours. After this reaction time, excess thionyl chloride and carbon tetrachloride were distilled off under a waterpump vacuum. Last residues of solvent were removed by brief incipient distillation under 2 mm Hg at a bath temperature of 60° C. 19.4 g (95% of theory) of 2,2-dimethyl-3-(2-chloro-2-(4-trifluoromethoxy-phenyl)-vinyl)-cyclopropanecarboxylic acid chloride were obtained as an oily liquid.

1. temperatureThe mixture was then heated to the reflux temperature for 4 hours
2. distillationAfter this reaction time, excess thionyl chloride and carbon tetrachloride were distilled off under a waterpump vacuum
3. customLast residues of solvent were removed by brief incipient distillation under 2 mm Hg at a bath temperature of 60° C