Water → Triphenylsulfonium (8-hydroxyoctyloxycarbonyl)difluoromethanesulfonate

Participants

Reaction Steps

30.0 parts of TPS-1, 20.0 parts of octane-1,8-diol, 2.2 parts of diphenylammonium triflate and 210 parts of monochlorobenzene were mixed and the resultant mixture was stirred at 80° C. to effect reaction. After completion of the reaction, the reaction mixture was concentrated to remove monochlorobenzene. Chloroform was added to the concentrate obtained and ion-exchanged water was added thereto. A chloroform layer was separated. After repeatedly washing the chloroform layer with ion-exchange water, 4.2 parts of active carbon was added to the chloroform layer obtained to stir for 1 hour. The chloroform layer was filtered and concentrated to obtain pale yellow oily matters. Tetrahydrofuran was added to the oily matters to stir. The mixture was filtered and the filtrate obtained was concentrated. Ethyl acetate was added to the concentrate obtained and the resultant mixture was stirred to conduct decantation. After repeating this operation, the residue was concentrated to obtain 19.5 parts of triphenylsulfonium (8-hydroxyoctyloxycarbonyl)difluoromethanesulfonate in the form of pale yellow oil, which is called as TPS-5.

Provenance & Evidence