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Ethanol → HCID 19836381, 화합물

HRID 1584000
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HRID 1584000 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([O:10][C:11]([F:16])([F:15])[CH:12]([F:14])[F:13])=[CH:6][CH:5]=1)([O-])=O.[CH2:17]([OH:19])[CH3:18]>[Pd]>[F:15][C:11]([F:16])([O:10][C:7]1[CH:8]=[CH:9][C:4]([NH:1][C:17](=[O:19])[CH3:18])=[CH:5][CH:6]=1)[CH:12]([F:14])[F:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 702EthanolHCID 119893Benzene, 1-nitro-4-(1,1,2,2-tetrafluoroethoxy)-

생성물 1

HCID 19836381HCID 19836381, 화합물수율 97%

시약·촉매·용매 1

HCID 23938Palladium촉매

실험 절차

55 g of 1-nitro-4-(1,1,2,2-tetrafluoroethoxy)benzene are hydrogenated in 300 ml of ethanol on 0.5 g of 10% strength palladium-on-charcoal in a circulatory hydrogenation apparatus under atmospheric pressure at 20°-45° C. for 1 h, the catalyst is filtered off and the solution is concentrated at 40° C. in vacuo. The 4-(1,1,2,2-tetrafluoroethoxy)aniline is diluted with 100 ml of glacial acetic acid, 23 ml of acetic anhydride are added dropwise at room temperature, 2 ml of water are added after 30 min., the solution is concentrated in vacuo at 50° C. after a short time and 500 ml of ice-water are added. 56 g (97%) of N-[4-(1,1,2,2-tetrafluoroethoxy)phenyl]-acetamide of m.p. 121°-122° C. are obtained.

후처리

  1. filtrationthe catalyst is filtered off
  2. concentrationthe solution is concentrated at 40° C. in vacuo
  3. additionThe 4-(1,1,2,2-tetrafluoroethoxy)aniline is diluted with 100 ml of glacial acetic acid, 23 ml of acetic anhydride
  4. additionare added dropwise at room temperature
  5. addition2 ml of water are added after 30 min.
  6. concentrationthe solution is concentrated in vacuo at 50° C. after a short time and 500 ml of ice-water
  7. additionare added

출처 및 근거

ORD 기록
ord-b5849e066c4841718d338dd919e3f55c
출처 데이터셋
uspto-grants-1985_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04555518

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