HCID 57656231, Verbindung → HCID 57656601, Verbindung

HRID 2041458Notizen

Reaktionsgleichung

[C:1]([O:5][C:6]([NH:8][CH2:9][C:10]1[CH:15]=[CH:14][C:13]([CH:16]([OH:22])[CH2:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[CH:12][C:11]=1[F:23])=[O:7])([CH3:4])([CH3:3])[CH3:2]>O1CCOCC1.[O-2].[O-2].[Mn+4]>[C:1]([O:5][C:6]([NH:8][CH2:9][C:10]1[CH:15]=[CH:14][C:13]([C:16](=[O:22])[CH2:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[CH:12][C:11]=1[F:23])=[O:7])([CH3:4])([CH3:2])[CH3:3]

Komponenten

Reaktionsbedingungen

Temperatur: 70 °C

Versuchsvorschrift

Add manganese dioxide (4.4 g, 50.6 mmol) to a solution of N-(tert-butoxycarbonyl)-2-fluoro-4-(1-hydroxy-3,3-dimethyl-butyl)-benzylamine (1.1 g, 3.38 mmol) in anhydrous 1,4-dioxane (45 mL) at room temperature. Heat the reaction mixture at 70° C. overnight. Filter the reaction mixture over Celite® and concentrate in vacuo. Purify by chromatography on silica gel eluting with hexane/EtOAc (9:1) to obtain the desired intermediate as an oil (980 mg, 90%).

Aufarbeitung

filtrationFilter the reaction mixture over Celite®
concentrationconcentrate in vacuo
customPurify by chromatography on silica gel eluting with hexane/EtOAc (9:1)

Quellen und Nachweise

ORD-Eintrag: ord-ffbde2569f254d7280d225bb1c78d236
Quelldatensatz: uspto-grants-2013_11
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US08580780B2

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