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Hydrochloric Acid → 2-Fluoro-4-(1,1,2,2-tetrafluoroethoxy)aniline

HRID 466798
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HRID 466798 반응식
C([NH:4][C:5]1[CH:10]=[CH:9][C:8]([O:11][C:12]([F:17])([F:16])[CH:13]([F:15])[F:14])=[CH:7][C:6]=1[F:18])(=O)C.Cl.C(=O)([O-])O.[Na+]>>[F:18][C:6]1[CH:7]=[C:8]([O:11][C:12]([F:16])([F:17])[CH:13]([F:15])[F:14])[CH:9]=[CH:10][C:5]=1[NH2:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 147216944-Acetylamino-3-fluoro-1-(1,1,2,2-tetrafluoroethoxy)benzene

생성물 1

HCID 146245342-Fluoro-4-(1,1,2,2-tetrafluoroethoxy)aniline수율 81%

실험 절차

0.60 Gram of 4-acetylamino-3-fluoro-1-(1,1,2,2-tetrafluoroethoxy)benzene and 10 ml of a 20% aqueous hydrochloric acid were added to a reactor and stirred under reflux for 2 hours. After cooling the reaction solution, a 5% aqueous sodium hydrogencarbonate solution was added to make the solution weakly alkaline. The reaction solution was then extracted with two 100-ml portions of diethyl ether. The ether layers were combined, dried and concentrated to obtain a yellow oily product as a residue. This oily product was subjected to chromatography on silica gel to obtain 0.40 g of 2-fluoro-4-(1,1,2,2-tetrafluoroethoxy)aniline.

후처리

  1. temperatureunder reflux for 2 hours
  2. temperatureAfter cooling the reaction solution
  3. extractionThe reaction solution was then extracted with two 100-ml portions of diethyl ether
  4. customdried
  5. concentrationconcentrated
  6. customto obtain a yellow oily product as a residue

출처 및 근거

ORD 기록
ord-585d398ab87348a1abef7e589bc3f6bf
출처 데이터셋
uspto-grants-1992_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05157155

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