Methanol → HCID 11359478, Verbindung

HRID 1870252Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1870252
C([O:4][CH2:5][C@H:6]1[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=2[N:10]([S:17]([C:20]2[CH:25]=[CH:24][C:23]([CH3:26])=[CH:22][CH:21]=2)(=[O:19])=[O:18])[CH2:9][CH2:8][CH2:7]1)(=O)C.C(=O)([O-])[O-].[K+].[K+].CO>O>[OH:4][CH2:5][C@@H:6]1[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=2[N:10]([S:17]([C:20]2[CH:21]=[CH:22][C:23]([CH3:26])=[CH:24][CH:25]=2)(=[O:19])=[O:18])[CH2:9][CH2:8][CH2:7]1

Komponenten

5

Edukt 3

HCID 887MethanolHCID 11430Potassium CarbonateHCID 11211019HCID 11211019, Verbindung

Produkt 1

HCID 11359478HCID 11359478, VerbindungAusbeute 100,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of (5R)-5-acetyloxymethyl-1-(p-toluenesulfonyl)-2,3,4,5-tetrahydro-1H-benzazepine (1.49 g), potassium carbonate (1.11 g) and methanol (15 ml) is stirred at room temperature for 20 minutes. The reaction solution is poured into water, and the mixture is extracted with dichloromethane. The extract is dried over sodium sulfate, and concentrated under reduced pressure to give (5S)-5-hydroxymethyl-1-(p-toluenesulfonyl)-2,3,4,5-tetrahydro-1H-benzazepine (1.33 g).

Aufarbeitung

  1. extractionthe mixture is extracted with dichloromethane
  2. dry with materialThe extract is dried over sodium sulfate
  3. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-55f9c65b54c04603b4471407661c3dae
Quelldatensatz
uspto-grants-2000_08
Patentnummer
US06096736

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