反应详情

A two-necked flask having a dry ice condenser fitted on top was charged with 50 ml of dry dimethylformamide and 2 g of a 60% strength by weight suspension of sodium hydride in paraffin, and subsequently 7.3 g of 4-chlorothiophenol in 10 ml of dimethylformamide were added dropwise. Chlorotrifluoroethane was then passed in at a reaction temperature of about 60° C., until the gas began to condense in the dry ice condenser. The mixture was stirred for a further 5 hours and the course of the reaction was monitored by thin-layer chromatography (silica gel; ethyl acetate/petroleum ether 1/5). The reaction mixture was worked up by pouring into water and extracting with dichloromethane. The combined organic extracts were dried and the solvent was distilled off at reduced pressure. The oily residue was subsequently distilled (43°-45° C./0.1 mbar), giving 8.8 g of 4-chloro(2',2',2'-trifluoroethylthio)benzene

1. customA two-necked flask having
2. customa dry ice condenser fitted on top
3. additionwere added dropwise
4. customwas then passed in at a reaction temperature of about 60° C., until the gas
5. extractionextracting with dichloromethane
6. customThe combined organic extracts were dried
7. distillationthe solvent was distilled off at reduced pressure
8. distillationThe oily residue was subsequently distilled (43°-45° C./0.1 mbar)