Diphenyl Ether → (4-Phenoxyphenyl)diphenylsulfonium

HRID 2212623노트

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HRID 2212623 반응식
[C:1]1([S:7]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:15]1([O:21][C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.FC(F)(F)C(OC(=O)C(F)(F)F)=O.[F:41][C:42]([F:48])([F:47])[S:43]([OH:46])(=[O:45])=[O:44]>ClCCl>[F:41][C:42]([F:48])([F:47])[S:43]([O-:46])(=[O:45])=[O:44].[C:9]1([S+:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[C:25]2[CH:24]=[CH:23][C:22]([O:21][C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=3)=[CH:27][CH:26]=2)[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1

참가 물질

6

반응물 4

HCID 7583Diphenyl EtherHCID 9845Trifluoroacetic anhydrideHCID 13679Diphenyl sulfoxideHCID 62406Trifluoromethanesulfonic acid

생성물 1

HCID 16213833(4-Phenoxyphenyl)diphenylsulfonium수율 38%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

In 100 ml of dichloromethane were dissolved 10.1 g (0.05 mol) of diphenylsulfoxide and 8.51 g (0.05 mol) of diphenyl ether, and 12.6 g (0.06 mol) of trifluoroacetic anhydride was added thereto at 0° C. Then 7.5 g (0.05 mol) of trifluoromethanesulfonic acid was added dropwise thereto at 0 to 5° C., followed by gradually warming to room temperature and reacting for 2 hours with stirring. After completion of the reaction, the reaction solution was washed with 100 ml of water five times and concentrated under reduced pressure, followed by purifying the resulting crude product by a column chromatography to obtain 9.59 g (Yield: 38%) of diphenyl-4-phenoxyphenylsulfonium trifluoromethanesulfonate as a yellow oily substance.

후처리

  1. additionwas added
  2. customat 0° C
  3. customat 0 to 5° C.
  4. customAfter completion of the reaction
  5. washthe reaction solution was washed with 100 ml of water five times
  6. concentrationconcentrated under reduced pressure
  7. customby purifying the resulting crude product by a column chromatography

출처 및 근거

ORD 기록
ord-a06f3be8d44d47b38d7c49812f147533
출처 데이터셋
uspto-grants-2006_09
특허 번호
US07101918B2

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