Water → 4-(4-Aminophenoxy)-2-butylaminopyridine

HRID 853311Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 853311
[NH2:1][C:2]1[CH:20]=[CH:19][C:5]([O:6][C:7]2[CH:12]=[CH:11][N:10]=[C:9]([NH:13][C:14](=O)[CH2:15][CH2:16][CH3:17])[CH:8]=2)=[CH:4][CH:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O>O1CCCC1>[NH2:1][C:2]1[CH:20]=[CH:19][C:5]([O:6][C:7]2[CH:12]=[CH:11][N:10]=[C:9]([NH:13][CH2:14][CH2:15][CH2:16][CH3:17])[CH:8]=2)=[CH:4][CH:3]=1

Komponenten

5

Edukt 3

HCID 962WaterHCID 21226445Aluminium lithium hydrideHCID 229364634-(4-Aminophenoxy)-2-butyrylaminopyridine

Produkt 1

HCID 229369234-(4-Aminophenoxy)-2-butylaminopyridine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

After dissolving 80 mg of 4-(4-aminophenoxy)-2-butyrylaminopyridine in 8 ml of tetrahydrofuran, 67 mg of lithium aluminum hydride was added while stirring at room temperature, and the mixture was stirred at 70° C. for 10 minutes. Water was added, extraction was performed with ethyl acetate, and then silica gel was added to the extract and the solvent was distilled off under reduced pressure. The silica gel was charged into a dry column packed with silica gel and purified by column chromatography (ethyl acetate) to obtain 54 mg of the target substance as a brown oil.

Aufarbeitung

  1. additionwas added
  2. stirringthe mixture was stirred at 70° C. for 10 minutes
  3. extractionextraction
  4. additionsilica gel was added to the
  5. extractionextract
  6. distillationthe solvent was distilled off under reduced pressure
  7. additionThe silica gel was charged into a dry column
  8. custompurified by column chromatography (ethyl acetate)
  9. customto obtain 54 mg of the target substance as a brown oil

Quellen und Nachweise

ORD-Eintrag
ord-a4efd87955d043029479ecb6212cb17c
Quelldatensatz
uspto-grants-2007_08
Patentnummer
US07253286B2

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