1-(3-Chloro-4-nitrophenyl)ethanone → 3'-(2,4-Difluorophenylthio)-4'-nitroacetophenone

HRID 1087192ノート

反応式

HRID 1087192 の反応式
Cl[C:2]1[CH:3]=[C:4]([C:11](=[O:13])[CH3:12])[CH:5]=[CH:6][C:7]=1[N+:8]([O-:10])=[O:9].[F:14][C:15]1[CH:21]=[C:20]([F:22])[CH:19]=[CH:18][C:16]=1[S-:17].[K+]>C1(C)C(C)=CC=CC=1>[F:14][C:15]1[CH:21]=[C:20]([F:22])[CH:19]=[CH:18][C:16]=1[S:17][C:2]1[CH:3]=[C:4]([C:11](=[O:13])[CH3:12])[CH:5]=[CH:6][C:7]=1[N+:8]([O-:10])=[O:9]

参加物

4

反応物 2

HCID 104427551-(3-Chloro-4-nitrophenyl)ethanoneHCID 23700122Potassium 2,4-difluorothiophenoxide

生成物 1

HCID 102448083'-(2,4-Difluorophenylthio)-4'-nitroacetophenone収率 61.8%

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

実験手順

A mixture of 3'-chloro-4'-nitroacetophenone (2.4 g), potassium 2,4-difluorothiophenoxide (2.7 g), and N,Ndimethylformamide (5 ml) in xylene (50 ml) was stirred for 8 hours at room temperature. The mixture was poured into ice-water and extracted with ethyl acetate. The extract was washed with water, dried over magnesium sulfate, and concentrated under reduced pressure. The residual solid was recrystallized from ethanol to give prisms of 3'-(2,4-difluorophenylthio)-4'-nitroacetophenone (2.3 g).

後処理

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with water
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residual solid was recrystallized from ethanol

出典と根拠

ORDレコード
ord-32a801e5fbff4ed1a50c02c93b95d056
出典データセット
uspto-grants-1991_07
特許番号
US05034417

反応ノート

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