Hydrochloric Acid → HCID 178489134, Verbindung
Reaktionsgleichung
F[C:2]1[C:7]([C:8]([F:11])([F:10])[F:9])=[CH:6][CH:5]=[CH:4][C:3]=1[C:12]([C:14]1[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=1)=O.O.[NH2:23][NH2:24].CCOC(C)=O.Cl>N1C=CC=CC=1.CN(C)C1C=CN=CC=1>[CH3:21][O:20][C:17]1[CH:18]=[CH:19][C:14]([C:12]2[C:3]3[C:2](=[C:7]([C:8]([F:11])([F:10])[F:9])[CH:6]=[CH:5][CH:4]=3)[NH:24][N:23]=2)=[CH:15][CH:16]=1Komponenten
7
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Reaktionsbedingungen
- Temperatur
- 100 °C
Versuchsvorschrift
(2-Fluoro-3-trifluoromethyl-phenyl)-(4-methoxy-phenyl)-methanone (59.6 mg, 0.2 mmol) was dissolved in 1 ml of pyridine. Hydrazine hydrate (97 μl, 2 mmol) and 4-(dimethylamino)-pyridine (24.4 mg, 0.2 mmol) were added. The reaction mixture was stirred overnight at 100° C. After cooling to room temperature, EtOAc and 1M HCl were added. The organic phase was washed three times with brine, dried over MgSO4 and concentrated under vacuum. Purification of the crude product by flash column chromatography on silica gel (n-heptane/ethyl acetate, 85:15) afforded 56 mg of the analytically pure product.
Aufarbeitung
- temperatureAfter cooling to room temperature
- washThe organic phase was washed three times with brine
- dry with materialdried over MgSO4
- concentrationconcentrated under vacuum
- customPurification of the crude product by flash column chromatography on silica gel (n-heptane/ethyl acetate, 85:15)
- customafforded 56 mg of the analytically pure product
Quellen und Nachweise
- ORD-Eintrag
- ord-e5b002c7829a48b59466c67f9f54788a
- Quelldatensatz
- uspto-grants-2009_09
- Patentnummer
- US07592363B2
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