Sulfuric Acid → HCID 17989209, compound

Participants

Reaction Conditions

Reaction Steps

16.7.8 g (93.97 mmol) of 3-chloro-2,6-difluoroanisole is dissolved in 800 ml of toluene. After 25.97 g (375.88 mmol) of isobutyronitrile is added, 283.97 ml (140.95 mmol) of a 0.5 molar solution of potassium hexamethyl disilazide in toluene is added in drops. The temperature in this case increases to 28° C. The batch is stirred for seven days at 60° C. After mixing with water and ethyl acetate, the reaction mixture is brought to a pH of 4 with 1 M sulfuric acid. After being extracted twice with ethyl acetate, the combined organic extracts are washed with water and with saturated NaCl solution and dried. After spinning-in and chromatography on silica gel (mobile solvent ethyl acetate/hexane), 7.46 g (21.4%) of the desired compound is obtained.

Provenance & Evidence