Sodium → HCID 24755562, compound

Participants

Reaction Steps

10 Parts of sodium slat of 4-oxo-1-adamantyl difluorosulfoacetate (purity: 55.2%) was charged in a vessel, and a mixed solvent of 30 parts of acetonitrile and 20 parts of ion-exchanged water was added thereto to give a mixture. A solution prepared by mixing 5.0 parts of 1-(2-oxo-2-phenylethyl)tetrahydrothiophenium bromide, 10 parts of acetonitrile and 20 parts of ion exchanged water was added to the mixture. After stirred for 15 hours, the stirred mixture was concentrated and extracted with 98 parts of chloroform. The organic layer was washed with ion-exchanged water. The obtained organic layer was concentrated. The concentrate was washed with 70 parts of ethyl acetate and the solvent was decanted and the crystals was dried to obtain 5.2 parts of 1-(2-oxo-2-phenylethyl)tetrahydrothiophenium 4-oxo-1-adamantyloxycarbonyldifluoromethanesulfonate in the form of white solid, which is called as acid generator B3.

Provenance & Evidence