(p-Hydroxyphenyl)diphenylsulfonium trifluoromethanesulfonate → Bicyclo[2.2.1]heptane-2-carboxylic acid-2,2-difluoro-2-sulfo-ethyl ester diphenyl-4-hydroxyphenylsulfonium salt

Participants

Reaction Steps

About 10 g of the diphenyl-4-hydroxyphenylsulfonium trifluoromethanesulfonate salt manufactured in the synthesis example 3 and about 10 g of a bicyclo[2.2.1]heptane-2-carboxylic acid-2,2-difluoro-2-sulfo-ethyl ester sodium salt were dissolved in about 100 ml of MC and about 100 ml of water, and a synthesis reaction (see Equation 4 below) was performed while stirring for about three hours. In this instance, a process of the synthesis reaction was observed by 19F NMR using a small amount of an extracted organic phase. The organic phase was extracted when the synthesis reaction was terminated, a solvent was removed, and the organic phase was washed using an MC of a soluble solvent and hexane of a sparingly soluble solvent. Next, the solvents were removed, and drying under a reduced pressure was performed to obtain about 9.42 g of a bicyclo[2.2.1]heptane-2-carboxylic acid-2,2-difluoro-2-sulfo-ethyl ester diphenyl-4-hydroxyphenylsulfonium salt, and a structure of the bicyclo[2.2.1]heptane-2-carboxylic acid-2,2-difluoro-2-sulfo-ethyl ester diphenyl-4-hydroxyphenylsulfonium salt was observed by 1H-NMR:

Provenance & Evidence