Hydroxyamine hydrochloride → HCID 136393701, Verbindung

HRID 1788889Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1788889
C([O-])(=O)C.[Na+].Cl.[NH2:7][OH:8].[CH2:9]([O:11][C:12](=[O:26])[C:13](=O)[C:14]1[C:22]2[C:17](=[C:18]([CH2:23][CH3:24])[CH:19]=[CH:20][CH:21]=2)[NH:16][CH:15]=1)[CH3:10]>O.C(O)C>[CH2:9]([O:11][C:12](=[O:26])[C:13](=[N:7][OH:8])[C:14]1[C:22]2[C:17](=[C:18]([CH2:23][CH3:24])[CH:19]=[CH:20][CH:21]=2)[NH:16][CH:15]=1)[CH3:10]

Komponenten

6

Edukt 3

HCID 443297Hydroxyamine hydrochlorideHCID 517045Sodium AcetateHCID 14010219ethyl 2-(7-ethyl-1H-indol-3-yl)-2-oxoacetate

Produkt 1

HCID 136393701HCID 136393701, VerbindungAusbeute 75,7 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel2×

Versuchsvorschrift

Solutions of sodium acetate (43.7 g, 0.53 mol) in water (100 mL) and hydroxylamine hydrochloride (37 g, 0.53 mol) in water (100 mL) were added to 7-ethyl-α-oxo-1H-indole-3-acetic acid ethyl ester 4 (17.4 g, 0.07 mol), in ethanol (250 mL) and the mixture was heated at reflux for 12 hours. The ethanol was removed by distillation and the resultant precipitate was filtered and recrystalized from hot ethanol to give the product (13.8 g, 75%), m.p. 167°-169° C. as a mixture of isomers.

Aufarbeitung

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 12 hours
  3. customThe ethanol was removed by distillation
  4. filtrationthe resultant precipitate was filtered
  5. customrecrystalized from hot ethanol

Quellen und Nachweise

ORD-Eintrag
ord-589aecb4d1ef418abc0ff082e9f786cc
Quelldatensatz
uspto-grants-1987_08
Patentnummer
US04686213

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