Sodium Hydroxide → HCID 21914127, Verbindung

HRID 887932Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 887932
C([N:4]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH2:6][CH:5]1[C:13]1[N:17]=[C:16]([CH2:18][CH2:19][CH3:20])[NH:15][N:14]=1)(=O)C.[OH-].[Na+]>C(O)C.C(OCC)(=O)C>[CH2:18]([C:16]1[NH:15][N:14]=[C:13]([CH:5]2[CH2:6][C:7]3[C:12](=[CH:11][CH:10]=[CH:9][CH:8]=3)[NH:4]2)[N:17]=1)[CH2:19][CH3:20]

Komponenten

5

Edukt 2

HCID 14798Sodium HydroxideHCID 21914092HCID 21914092, Verbindung

Produkt 1

HCID 21914127HCID 21914127, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

A solution of the compound 91 (0.42 g) in ethanol (25 ml) was treated with an aqueous NaOH solution (3 M, 25 mL) and the reaction mix was refluxed for 24 hours. The reaction was cooled, diluted with ethyl acetate, and treated with cold distilled water. The layers were separated and the aqueous fraction was extracted 5 times with ethyl acetate and the combined organic fractions were dried, concentrated and purified by preparatory column chromatography yielding 2,3-dihydro-2-(5-propyl-1H-1,2,4-triazol-3-yl)-1H-indole.

Aufarbeitung

  1. additionthe reaction mix
  2. temperaturewas refluxed for 24 hours
  3. temperatureThe reaction was cooled
  4. additiontreated
  5. distillationwith cold distilled water
  6. customThe layers were separated
  7. extractionthe aqueous fraction was extracted 5 times with ethyl acetate
  8. customthe combined organic fractions were dried
  9. concentrationconcentrated
  10. custompurified by preparatory column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-8f289a655286477cba3d088e1160d624
Quelldatensatz
uspto-grants-2012_08
Patentnummer
US08247432B2

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