Potassium Carbonate → HCID 59164777, Verbindung

HRID 1441726

Reaktionsgleichung

Reaktionsgleichung von HRID 1441726
F[C:2]1[CH:9]=[C:8]([N+:10]([O-:12])=[O:11])[CH:7]=[CH:6][C:3]=1[CH:4]=O.Cl.[C:14]([NH2:17])(=[NH:16])[CH3:15].C([O-])([O-])=O.[K+].[K+]>C(#N)C>[CH3:15][C:14]1[N:17]=[CH:4][C:3]2[C:2](=[CH:9][C:8]([N+:10]([O-:12])=[O:11])=[CH:7][CH:6]=2)[N:16]=1

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 67170Acetamidine monohydrochlorideHCID 45629192-Fluoro-4-nitrobenzaldehyde

Produkt 1

HCID 59164777HCID 59164777, VerbindungAusbeute 34,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Reaktionsbedingungen

Temperatur
25 °C

Versuchsvorschrift

2-Fluoro-4-nitrobenzaldehyde (1.00 g, 5.92 mmol) and acetamidine hydrochloride (0.783 g, 8.28 mmol) were added to a suspension of activated 4 Å MS (1.2 g) in acetonitrile (60 mL). K2CO3 (1.14 g, 8.28 mmol) was then added and the reaction was heated to reflux for 4 h. The reaction was then cooled to 25° C. and filtered through celite rinsing with CH2Cl2. The crude product was purified by flash chromatography on silica eluting with 0-10% acetone in CH2Cl2 to give 0.386 g of compound 25A as a yellow solid.

Aufarbeitung

  1. temperaturethe reaction was heated
  2. temperatureto reflux for 4 h
  3. filtrationfiltered
  4. washthrough celite rinsing with CH2Cl2
  5. customThe crude product was purified by flash chromatography on silica eluting with 0-10% acetone in CH2Cl2

Quellen und Nachweise

ORD-Eintrag
ord-6049b3b6053640fbb4e80b2dc4f7fbbb
Quelldatensatz
uspto-grants-2010_02
Patentnummer
US07655688B2

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