Acetic Acid → HCID 69063437, Verbindung

HRID 730431Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 730431
[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][C:22]([F:25])=[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][C:22]([F:25])=[CH:21][CH:20]=2)=[CH:15][CH:16]=1

Komponenten

5

Edukt 3

HCID 176Acetic AcidHCID 109550394-Fluoro-alpha-(4-fluorophenyl)benzenemethanamineHCID 86606793HCID 86606793, Verbindung

Produkt 1

HCID 69063437HCID 69063437, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

To a solution of formyl succinonitrile potassium salt (6.67 g, 45.6 mmol) and 1,1-bis(4-fluorophenyl) methaneamine (11.0 g, 50.2 mmol) in water (19 ml) was added acetic acid (19 ml) at room temperature, and the mixture was stirred 100° C. for 30 minutes. The solvent was distilled off under reduced pressure. The residue was poured into iced water, made basic with potassium carbonate and then extracted with ethyl acetate. The extract was washed with water and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure to give the objective product as oily matter. Yield (amount) 14.0 g, yield (rate) 99.3%

Aufarbeitung

  1. distillationThe solvent was distilled off under reduced pressure
  2. additionThe residue was poured into iced water
  3. extractionextracted with ethyl acetate
  4. washThe extract was washed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. customto give the objective product as oily matter
  8. customYield (amount) 14.0 g
  9. customyield (rate) 99.3%

Quellen und Nachweise

ORD-Eintrag
ord-96fc6d4be570439583138995162dc8a3
Quelldatensatz
uspto-grants-2009_09
Patentnummer
US07582651B2

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