Water → N-(4-Fluorophenyl)-N'-(4-{[2-(2-oxotetrahydro-1H-1-pyrrolyl)-4-pyridyl]oxy}phenyl)urea

HRID 1010204Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1010204
[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]([NH:11][C:12]2[CH:17]=[CH:16][C:15]([O:18][C:19]3[CH:24]=[CH:23][N:22]=[C:21]([NH:25][C:26](=[O:31])[CH2:27][CH2:28][CH2:29]Cl)[CH:20]=3)=[CH:14][CH:13]=2)=[O:10])=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].CN(C)C=O.O>C(OCC)(=O)C>[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]([NH:11][C:12]2[CH:17]=[CH:16][C:15]([O:18][C:19]3[CH:24]=[CH:23][N:22]=[C:21]([N:25]4[CH2:29][CH2:28][CH2:27][C:26]4=[O:31])[CH:20]=3)=[CH:14][CH:13]=2)=[O:10])=[CH:4][CH:3]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 22936908N-(4-Fluorophenyl)-N'-(4-{[2-(4-chlorobutyrylamino)-4-pyridyl]oxy}phenyl)urea

Produkt 1

HCID 22936528N-(4-Fluorophenyl)-N'-(4-{[2-(2-oxotetrahydro-1H-1-pyrrolyl)-4-pyridyl]oxy}phenyl)ureaAusbeute 40,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

N-(4-Fluorophenyl)-N′-(4-{[2-(4-chlorobutyrylamino)-4-pyridyl]oxy}phenyl)urea (56 mg), potassium carbonate (46 mg) and dimethylformamide (2 ml) were stirred at 150° C. for 15 minutes. Water and ethyl acetate were added for extraction, and the extract was passed through a glass filter coated with silica gel. The silica gel was washed with ethyl acetate, and the organic layer was distilled off under reduced pressure. Ethyl acetate and hexane were added to the residue, and the precipitated solid was filtered out to obtain 21 mg of a faint brown powder.

Aufarbeitung

  1. filtrationfilter
  2. washThe silica gel was washed with ethyl acetate
  3. distillationthe organic layer was distilled off under reduced pressure
  4. additionEthyl acetate and hexane were added to the residue
  5. filtrationthe precipitated solid was filtered out

Quellen und Nachweise

ORD-Eintrag
ord-f7193c14607b4e0ba1968e31cbdc7216
Quelldatensatz
uspto-grants-2011_07
Patentnummer
US07973160B2

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