Triethylamine → 3-Methyl 1-(4-nitrophenyl) 5-[4-(trifluoromethyl)phenyl]piperidine-1,3-dicarboxylate
Reaktionsgleichung
[F:1][C:2]([F:20])([F:19])[C:3]1[CH:8]=[CH:7][C:6]([CH:9]2[CH2:14][NH:13][CH2:12][CH:11]([C:15]([O:17][CH3:18])=[O:16])[CH2:10]2)=[CH:5][CH:4]=1.C(N(CC)CC)C.[C:28](Cl)(=[O:39])[O:29][C:30]1[CH:35]=[CH:34][C:33]([N+:36]([O-:38])=[O:37])=[CH:32][CH:31]=1>ClCCl>[F:20][C:2]([F:19])([F:1])[C:3]1[CH:8]=[CH:7][C:6]([CH:9]2[CH2:14][N:13]([C:28]([O:29][C:30]3[CH:31]=[CH:32][C:33]([N+:36]([O-:38])=[O:37])=[CH:34][CH:35]=3)=[O:39])[CH2:12][CH:11]([C:15]([O:17][CH3:18])=[O:16])[CH2:10]2)=[CH:5][CH:4]=1Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 0 °C
Versuchsvorschrift
20.0 g (69.6 mmol) of the compound from Example 53A were dissolved in 1.0 l of dichloromethane, and 14.1 g (139 mmol) of triethylamine were added at 0° C. 14.0 g (69.6 mmol) of 4-nitrophenyl chlorocarbonate were then added dropwise. The reaction mixture was stirred at 0° C. for 2 h and then at RT for 16 h. For workup, the mixture was washed with saturated aqueous sodium bicarbonate solution. The organic phase was dried over magnesium sulphate, filtered and concentrated under reduced pressure. This gave 31.3 g of crude product, which was reacted without any further purification steps.
Aufarbeitung
- waitat RT for 16 h
- washFor workup, the mixture was washed with saturated aqueous sodium bicarbonate solution
- dry with materialThe organic phase was dried over magnesium sulphate
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThis gave 31.3 g of crude product, which was reacted without any further purification steps
Quellen und Nachweise
- ORD-Eintrag
- ord-1257b7c5762c46bd9a1c0c19d14b6878
- Quelldatensatz
- uspto-grants-2015_03
- Patentnummer
- US08987248B2
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