반응 #2021475

ord-cb9cd00415714cfdadc5e0a42fc263c9

반응 방정식

O=S(c1ccccc1)c1ccccc1
diphenylsulfoxide
Cc1ccccc1
toluene
O=C(OC(=O)C(F)(F)F)C(F)(F)F
trifluoroacetic anhydride
O=S(=O)(O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F
perfluorobutanesulfonic acid
Cc1ccc([S+](c2ccccc2)c2ccccc2)cc1.O=S(=O)([O-])C(F)(F)C(F)(F)C(F)(F)C(F)(F)F
4-methylphenyldiphenylsulfonium perfluorobutanesulfonate

반응 조건

온도
2°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축the lower layer was concentrated
  2. 2
    workup.ADDITIONdiluted with 100 parts of chloroform
  3. 3
    세척The obtained chloroform solution was washed 11 times with 50 parts of ion-exchange water
  4. 4
    농축concentrated

실험 절차

Into a four-necked flask were charged 5.06 parts of diphenylsulfoxide and 50.6 parts of toluene, and the mixture was cooled to 2° C. Then, 10.5 parts of trifluoroacetic anhydride and 7.50 parts of perfluorobutanesulfonic acid were added and the mixture was stirred at the same temperature for 60 minutes. After standing, the lower layer was concentrated and diluted with 100 parts of chloroform. The obtained chloroform solution was washed 11 times with 50 parts of ion-exchange water and concentrated to give 12.0 parts of 4-methylphenyldiphenylsulfonium perfluorobutanesulfonate, which is referred to herein as PAG4.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06383713B1uspto-grants-2002_05