Acetic Acid → 2-({[(4-Fluorophenyl)(phenyl)methyl]amino}methylidene)butanedinitrile

HRID 730423Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 730423
[K].[CH:2]([CH:4]([CH2:7][C:8]#[N:9])[C:5]#[N:6])=O.[F:10][C:11]1[CH:16]=[CH:15][C:14]([CH:17]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[NH2:18])=[CH:13][CH:12]=1.C(O)(=O)C>O>[F:10][C:11]1[CH:12]=[CH:13][C:14]([CH:17]([NH:18][CH:2]=[C:4]([CH2:7][C:8]#[N:9])[C:5]#[N:6])[C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[CH:15][CH:16]=1

Komponenten

5

Edukt 3

HCID 176Acetic AcidHCID 111832724-Fluoro-α-phenylbenzenemethanamineHCID 86606793HCID 86606793, Verbindung

Produkt 1

HCID 690558642-({[(4-Fluorophenyl)(phenyl)methyl]amino}methylidene)butanedinitrile

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

To a solution of formyl succinonitrile potassium salt (7.26 g, 49.7 mmol) and 1-(4-fluorophenyl)-1-phenylmethaneamine (11.0 g, 54.7 mmol) in water-(20 ml) was added acetic acid (20 ml) at room temperature, the mixture was stirred at 100° C. for 30 minutes, and the solvent was distilled off under reduced pressure. The residue was poured into iced water, made basic by adding potassium carbonate and then extracted with ethyl acetate. The extract was washed with water, dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to give the objective product as a solid material.

Aufarbeitung

  1. distillationthe solvent was distilled off under reduced pressure
  2. additionThe residue was poured into iced water
  3. additionby adding potassium carbonate
  4. extractionextracted with ethyl acetate
  5. washThe extract was washed with water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. distillationThe solvent was distilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-3fbc576e9c1547baab609e75c9ee59f5
Quelldatensatz
uspto-grants-2009_09
Patentnummer
US07582651B2

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