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4-Fluoro-3-methoxyaniline → HCID 23284696、化合物

HRID 369247
ノート
印刷プレビュー

反応式

HRID 369247 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 23284696HCID 23284696、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
90 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a7ec8c2365cb461484695ae3ac638dbf
出典データセット
uspto-grants-2000_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06136823

反応ノート

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