반응 #1909799

ord-bf0ea37fc3f84725a4d5ad4ed5578627

반응 방정식

O=C1OCC(Sc2ccccc2)O1
4-Phenylsulfanyl-[1,3]dioxolan-2-one
O=S([O-])OO.[K+]
OXONE
O
water
O=C1OCC(S(=O)(=O)c2ccccc2)O1
4-benzenesulfonyl-[1,3]dioxolan-2-one

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The obtained reaction mixture
  2. 2
    workup.STIRRINGwas agitated at room temperature for 12 hours
  3. 3
    기타was removed
  4. 4
    workup.DISTILLATIONdecompression distillation
  5. 5
    추출the resulting product was extracted
  6. 6
    추출The extracted organic solvent layer was again extracted
  7. 7
    기타was removed
  8. 8
    기타organic solvent was removed
  9. 9
    workup.DISTILLATIONdecompression distillation
  10. 10
    기타Using silica gel chromatography, separation and purification

실험 절차

4-Phenylsulfanyl-[1,3]dioxolan-2-one) was dissolved in methanol, and OXONE® was added. The resulting mixture was agitated at room temperature for 5 minutes and water was added. The obtained reaction mixture was agitated at room temperature for 12 hours. From the agitated reaction mixture, methanol was removed using decompression distillation and the resulting product was extracted using methylene chloride. The extracted organic solvent layer was again extracted using water, moisture was removed using magnesium sulfate, and then organic solvent was removed using decompression distillation. Using silica gel chromatography, separation and purification were performed to obtain a pure target product, 4-benzenesulfonyl-[1,3]dioxolan-2-one.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07037624B2uspto-grants-2006_05