Ammonium formate → HCID 22380663, Verbindung

HRID 895647Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 895647
C(O[CH:5]([C:14]1[CH:19]=[CH:18][C:17]([C:20]2[O:21][CH2:22][C:23]([CH3:26])([CH3:25])[N:24]=2)=[CH:16][CH:15]=1)[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[O:12][CH3:13])(=O)C.C([O-])=O.[NH4+]>CO.[Pd]>[CH3:25][C:23]1([CH3:26])[CH2:22][O:21][C:20]([C:17]2[CH:18]=[CH:19][C:14]([CH2:5][C:6]3[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=3[O:12][CH3:13])=[CH:15][CH:16]=2)=[N:24]1

Komponenten

5

Edukt 2

HCID 2723923Ammonium formateHCID 223807461-[4-(4,4-Dimethyloxazolin-2-yl)phenyl]-1-(2-methoxyphenyl)methyl acetate

Produkt 1

HCID 22380663HCID 22380663, VerbindungAusbeute 73,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

In an amount of 23.5 mg of the 1-[4-(4,4-dimethyloxazolin-2-yl)phenyl]-1-(2-methoxyphenyl)methyl acetate obtained above was dissolved in methanol (0.47 ml), added with 10% palladium/carbon (24 mg) and ammonium formate (42 mg) under argon atmosphere and stirred at 60° C. for 2 hours. After insoluble matters were removed by filtration, the solvent was evaporated under reduced pressure. The residue was purified by preparative thin layer silica gel column chromatography (developing solvent: hexane:ethyl acetate=1:1) to obtain 14.4 mg of the title compound. Yield: 73%.

Aufarbeitung

  1. customAfter insoluble matters were removed by filtration
  2. customthe solvent was evaporated under reduced pressure
  3. customThe residue was purified by preparative thin layer silica gel column chromatography (developing solvent: hexane:ethyl acetate=1:1)

Quellen und Nachweise

ORD-Eintrag
ord-4576680ac5d542658cb4b108f8e82f1f
Quelldatensatz
uspto-grants-2005_07
Patentnummer
US06916822B2

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