Reaktionsgleichung
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:19]=[C:18]([N+:20]([O-])=O)[CH:17]=[CH:16][C:15]=2[O:23][C:24]([F:27])([F:26])[F:25])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]>C(OCC)(=O)C.C(O)(=O)C.[Pd]>[C:1]([O:5][C:6]([N:8]1[CH2:9][CH2:10][N:11]([C:14]2[CH:19]=[C:18]([NH2:20])[CH:17]=[CH:16][C:15]=2[O:23][C:24]([F:26])([F:27])[F:25])[CH2:12][CH2:13]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]Komponenten
5
Edukt 1
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 3
Versuchsvorschrift
0.41 g of 4-(5-Nitro-2-trifluoromethoxy-phenyl)-piperazine-1-carboxylic acid tert-butyl ester (1.055 mmol) were dissolved in 10 mL ethyl acetate and 10 mL acetic acid. 0.12 g 10% Palladium/charcoal were added and the mixture hydrogenated for 3 h at room temperature. The catalyst was filtered over Celite, washed with ethyl acetate and the combined filtrates evaporated to dryness. The residue was treated with water, the pH adjusted to 9-10 with 1 N aquous sodium hydroxide and the aquous phase extracted twice with dichloromethane. The combined organic extracts were dried over magnesium sulfate, filtered, and the solvent evaporated under reduced pressure to yield 0.372 g of the product.
Aufarbeitung
- filtrationThe catalyst was filtered over Celite
- washwashed with ethyl acetate
- customthe combined filtrates evaporated to dryness
- additionThe residue was treated with water
- extractionthe aquous phase extracted twice with dichloromethane
- dry with materialThe combined organic extracts were dried over magnesium sulfate
- filtrationfiltered
- customthe solvent evaporated under reduced pressure
Quellen und Nachweise
- ORD-Eintrag
- ord-2bedcfa7abc741f2aa34ba263ce6204c
- Quelldatensatz
- uspto-grants-2010_09
- Patentnummer
- US07790727B2
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