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

HRID 1087192노트

반응식

HRID 1087192 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-32a801e5fbff4ed1a50c02c93b95d056
출처 데이터셋
uspto-grants-1991_07
특허 번호
US05034417

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