p-Toluenesulfonic acid → HCID 56837185, compound

Participants

Reaction Steps

Catalytic p-toluenesulfonic acid is added to a mixture of 25 g of 4-(3-difluoromethoxyphenylthio)-2,5-xylidine (0.085 moles) and 141 ml of triethylorthoformiate (0.85 moles). The temperature is brought to reflux and the mixture is kept under stirring for 3 hours. The reaction trend is controlled with TLC (eluent hexane/ethyl acetate 8:2). When the reaction is completed, the mixture is concentrated at reduced pressure and the raw product obtained dissolved in methylene chloride (234 ml); 14.3 ml of N-ethylmethylamine (0.17 moles) are added dropwise. The mixture is kept under stirring for 3 hours at 40° C. and, after TLC control (eluent hexane/ethyl acetate 8:2), is concentrated at reduced pressure. 20 g of the desired product are obtained.

Provenance & Evidence