Anisole → HCID 23144325, Verbindung

HRID 1967764Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1967764
[O:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]1[N:7]=[C:8]([NH:17][C:18]([C:20]2[CH:25]=[CH:24][N:23]=[C:22]([O:26]CC3C=CC(OC)=CC=3)[CH:21]=2)=[O:19])[S:9][C:10]=1[C:11]1[CH:16]=[CH:15][N:14]=[CH:13][CH:12]=1.C1(OC)C=CC=CC=1.C(=O)([O-])O.[Na+]>FC(F)(F)C(O)=O>[O:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]1[N:7]=[C:8]([NH:17][C:18]([C:20]2[CH:25]=[CH:24][NH:23][C:22](=[O:26])[CH:21]=2)=[O:19])[S:9][C:10]=1[C:11]1[CH:12]=[CH:13][N:14]=[CH:15][CH:16]=1

Komponenten

5

Edukt 3

HCID 7519AnisoleHCID 516892Sodium BicarbonateHCID 23144506HCID 23144506, Verbindung

Produkt 1

HCID 23144325HCID 23144325, VerbindungAusbeute 68 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6422Trifluoroacetic acidLösungsmittel

Reaktionsbedingungen

Temperatur
65 °C

Versuchsvorschrift

Compound 106 (2.10 g, 4.33 mmol) and anisole (4.72 mL, 43.4 mmol) were suspended in trifluoroacetic acid (7 mL), followed by stirring at 65° C. for 30 minutes. A saturated aqueous solution of sodium hydrogencarbonate was added to the reaction mixture to adjust the pH to 8, and the precipitated solid was collected by filtration. The resulting solid was purified through silica gel column chromatography (chloroform:methanol=4:1) to afford the entitled Compound 112 (1.07 g, 68%).

Aufarbeitung

  1. filtrationthe precipitated solid was collected by filtration
  2. customThe resulting solid was purified through silica gel column chromatography (chloroform:methanol=4:1)

Quellen und Nachweise

ORD-Eintrag
ord-ce8e780b305542a88baf38e3aff0c9d1
Quelldatensatz
uspto-grants-2013_04
Patentnummer
US08420827B2

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