Water → 1-(2-Fluoro-5-methoxybenzylidene)-2-(4-fluorophenyl)hydrazine

HRID 13187

Reaktionsgleichung

Reaktionsgleichung von HRID 13187
[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][NH2:9])=[CH:4][CH:3]=1.[F:10][C:11]1[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][C:12]=1[CH:13]=O.C(=O)([O-])[O-].[Cs+].[Cs+].O>CN(C=O)C>[F:10][C:11]1[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][C:12]=1[CH:13]=[N:9][NH:8][C:5]1[CH:6]=[CH:7][C:2]([F:1])=[CH:3][CH:4]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 10796Cesium carbonateHCID 69982(4-Fluorophenyl)hydrazineHCID 27348722-Fluoro-5-methoxybenzaldehyde

Produkt 1

HCID 668125981-(2-Fluoro-5-methoxybenzylidene)-2-(4-fluorophenyl)hydrazine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

(4-fluorophenyl)hydrazine (6.5 g, 40 mmol), 2-fluoro-5-methoxybenzaldehyde (6.2 g, 40 mmol) and cesium carbonate (13 g, 40 mmol) were stirred in DMF (40 mL) at r.t. under argon atmosphere for 1.5 h and was then poured with stirring into water and extracted with ethyl acetate. The organic phase was washed trice with water, then brine and evaporated. The residue crystallized slowly to afford the subtitle compound as a beige-light brown crystal mass (10.21 g).

Aufarbeitung

  1. additionwas then poured
  2. extractionextracted with ethyl acetate
  3. washThe organic phase was washed trice with water
  4. custombrine and evaporated
  5. customThe residue crystallized slowly

Quellen und Nachweise

ORD-Eintrag
ord-5de05775b2444b41b706539db408683e
Quelldatensatz
uspto-grants-2010_06
Patentnummer
US07728030B2

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