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Ethanol → HCID 19836381、化合物

HRID 845524
ノート
印刷プレビュー

反応式

HRID 845524 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

HCID 19836381HCID 19836381、化合物収率 97%

試薬・触媒・溶媒 1

HCID 23938Palladium触媒

実験手順

55 g of 1-nitro-4-(1,1,2,2-tetrafluoroethoxy)-benzene are hydrogenated in 300 ml of ethanol over 0.5 g of 10% strength palladium-on-charcoal in a circulatory hydrogenation apparatus under atmospheric pressure at 20°-45° C. for 1 hour, the catalyst is filtered off and the solution is concentrated in vacuo at 40° C. 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 minutes, the solution is concentrated at 50° C. in vacuo after a short time and 500 ml of icewater are added. 56 g (97% of theoretical) of N-[4-(1,1,2,2-tetrafluoroethoxy)phenyl]-acetamide of m.p. 121°-122° C. are obtained.

後処理

  1. filtrationthe catalyst is filtered off
  2. concentrationthe solution is concentrated in vacuo at 40° C
  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 minutes
  6. concentrationthe solution is concentrated at 50° C. in vacuo after a short time and 500 ml of icewater
  7. additionare added

出典と根拠

ORDレコード
ord-e593f56e7a2945a58299822bd98360d7
出典データセット
uspto-grants-1988_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04758579

反応ノート

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