반응 #1438239

ord-300e9bdcb7c34c67839e90a34cbf56e3

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타transferred to a separatory funnel
  2. 2
    workup.STIRRINGshaken
  3. 3
    기타The water layer was removed
  4. 4
    workup.ADDITIONAfter the addition of 300 ml of distilled water
  5. 5
    workup.STIRRINGthe mixture was shaken
  6. 6
    기타The water layer was removed
  7. 7
    건조The dichloromethane solution was dried with anhydrous magnesium sulfate
  8. 8
    여과filtered
  9. 9
    기타After evaporating dichloromethane from the dried solution
  10. 10
    기타the residual liquid was dried under reduced pressure

실험 절차

26.7 g of tris(4-fluorophenyl)sulfonium trifluoromethanesulfonate was dissolved in 200 g of dichloromethane in a reaction flask, in which the atmosphere was replaced with nitrogen. 600 g of 10 wt % sodium hydroxide aqueous solution, 5.8 g of tetra-n-butylammonium bromide, and 20.1 g of n-butanethiol were added. The mixture was stirred for 30 minutes at room temperature and transferred to a separatory funnel, shaken, and allowed to stand still. The water layer was removed. After the addition of 300 ml of distilled water, the mixture was shaken and allowed to stand still. The water layer was removed. The dichloromethane solution was dried with anhydrous magnesium sulfate and filtered. After evaporating dichloromethane from the dried solution, the residual liquid was dried under reduced pressure to obtain 23.4 g of tris(4-n-butylthiophenyl)sulfonium trifluoromethanesulfonate.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07217492B2uspto-grants-2007_05