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Trifluoroacetic acid → HCID 86652488, 화합물

HRID 623393
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인쇄 미리보기

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HRID 623393 반응식
C([O-])(=O)C.C([O-])(=O)C.[CH3:9][O:10][C:11]1[CH:16]=[CH:15][C:14]([IH+:17])=[CH:13][CH:12]=1.[CH3:18][O:19][C:20]1[CH:25]=[CH:24][C:23]([IH+])=[CH:22][CH:21]=1.[F:27][C:28]([F:33])([F:32])[C:29]([OH:31])=[O:30].C1(OC)C=CC=CC=1>ClCCl>[F:27][C:28]([F:33])([F:32])[C:29]([O-:31])=[O:30].[CH3:9][O:10][C:11]1[CH:16]=[CH:15][C:14]([I+:17][C:23]2[CH:24]=[CH:25][C:20]([O:19][CH3:18])=[CH:21][CH:22]=2)=[CH:13][CH:12]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6422Trifluoroacetic acidHCID 7519AnisoleHCID 86652489HCID 86652489, 화합물

생성물 1

HCID 86652488HCID 86652488, 화합물수율 84.2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
-30 °C

실험 절차

Under N2 protection, 1.41 g (4 mmol) p-methoxyphenyliodonium diacetate was dissolved in 30 mL of dry dichloromethane and the solution was cooled to −30° C. 0.61 mL (8 mmol) of trifluoroacetic acid was added and the solution was slowly brought back to room temperature and stirred for 30 minutes. The solution was, again, cooled to −30° C. and 0.44 mL (4 mmol) anisole was added slowly and the mixture was warmed back up to room temperature and stirred for 1 hour. The solvent was evaporated and the residual solid was recrystallized from diethylether/dichloromethane to give 1.53 g bis(p-methoxyphenyl)iodonium trifluoroacetate (71%).

후처리

  1. customwas slowly brought back to room temperature
  2. temperatureagain, cooled to −30° C.
  3. temperaturethe mixture was warmed back up to room temperature
  4. stirringstirred for 1 hour
  5. customThe solvent was evaporated
  6. customthe residual solid was recrystallized from diethylether/dichloromethane

출처 및 근거

ORD 기록
ord-39d7f739463a443e9063ecacf1df2904
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09302990B2

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