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4-Fluoro-3-methoxyaniline → HCID 23284696, 화합물

HRID 369247
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HRID 369247 반응식
[F:1][C:2]1[CH:8]=[CH:7][C:5]([NH2:6])=[CH:4][C:3]=1[O:9][CH3:10].C(O[CH:14]=[C:15]([C:21](=[O:32])[C:22]1[CH:27]=[C:26]([F:28])[C:25]([F:29])=[C:24]([CH3:30])[C:23]=1F)[C:16]([O:18][CH2:19][CH3:20])=[O:17])C.F[C:34]1C(C)=C(F)C(F)=CC=1C(CC(OCC)=O)=O>C(Cl)(Cl)Cl>[F:28][C:26]1[CH:27]=[C:22]2[C:23](=[C:24]([CH3:30])[C:25]=1[F:29])[N:6]([C:5]1[CH:7]=[CH:8][C:2]([F:1])=[C:3]([O:9][CH2:10][CH3:34])[CH:4]=1)[CH:14]=[C:15]([C:16]([O:18][CH2:19][CH3:20])=[O:17])[C:21]2=[O:32]
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참가 물질

5

반응물 3

HCID 27745334-Fluoro-3-methoxyanilineHCID 14052572Ethyl 3-oxo-3-(2,4,5-trifluoro-3-methylphenyl)propanoateHCID 53656353HCID 53656353, 화합물

생성물 1

HCID 23284696HCID 23284696, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

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온도
90 °C

실험 절차

4-Fluoro-3-methoxyaniline (1.4 g) was added to a chloroform solution (10 ml) of ethyl 3-ethoxy-2-(2,4,5-trifluoro-3-methylbenzoyl)acrylate synthesized from ethyl 2,4,5-trifluoro-3-methylbenzoylacetate (2.6 g) in accordance with a method known per se in the art. The mixture was concentrated under reduced pressure, and anhydrous potassium carbonate (3.0 g) and N,N-dimethylformamide (7 ml) were added to the residue, followed by stirring at 90° C. for 15 minutes. The reaction mixture was allowed to cool, and chloroform (100 ml) and distilled water (250 ml) were added to the mixture, thereby conducting liquid separation. A chloroform layer was then washed twice with distilled water (250 ml), dried over anhydrous magnesium sulfate and concentrated under reduced pressure. Deposits were dispersed in ethanol, collected by filtration and washed with ethanol and diisopropyl ether in that order to obtain the title compound (2.59 g) as a colorless powder.

후처리

  1. concentrationThe mixture was concentrated under reduced pressure, and anhydrous potassium carbonate (3.0 g) and N,N-dimethylformamide (7 ml)
  2. additionwere added to the residue
  3. temperatureto cool
  4. distillationchloroform (100 ml) and distilled water (250 ml)
  5. additionwere added to the mixture
  6. customliquid separation
  7. washA chloroform layer was then washed twice with distilled water (250 ml)
  8. dry with materialdried over anhydrous magnesium sulfate
  9. concentrationconcentrated under reduced pressure
  10. additionDeposits were dispersed in ethanol
  11. filtrationcollected by filtration
  12. washwashed with ethanol and diisopropyl ether in that order

출처 및 근거

ORD 기록
ord-a7ec8c2365cb461484695ae3ac638dbf
출처 데이터셋
uspto-grants-2000_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06136823

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