반응 #645229

반응 방정식

sodium

difluorosulfoacetic acid-4-oxo-1-adamantyl ester

triphenylsulfonium chloride

→

triphenylsulfonium 4-oxo-1-adamantyloxycarbonyldifluromethanesulfonate

용매

water

acetonitrile

water

acetonitrile

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   농축concentrated
3. 3
   추출extracted with 142 parts of chloroform
4. 4
   세척The organic layer was washed with ion-exchanged water
5. 5
   농축the resulting organic layer was concentrated
6. 6
   세척The concentrate was washed with 24 parts of tert-butyl methyl ether

실험 절차

To 5.4 parts (35.6% purity) of the sodium salt of difluorosulfoacetic acid-4-oxo-1-adamantyl ester, a mixture of 16 parts of acetonitrile and 16 parts of ion-exchanged water was added. To the mixture, a solution of 1.7 parts of triphenylsulfonium chloride, 5 parts of acetonitrile, and 5 parts of ion-exchanged water was added. The resultant mixture was stirred for 15 hours, then concentrated, and extracted with 142 parts of chloroform. The organic layer was washed with ion-exchanged water, and the resulting organic layer was concentrated. The concentrate was washed with 24 parts of tert-butyl methyl ether, giving 1.7 parts of triphenylsulfonium 4-oxo-1-adamantyloxycarbonyldifluromethanesulfonate (B1) in the form of a white solid.

출처