Reaktionsgleichung
Br[C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][C:11]([O:14][CH2:15][CH2:16][CH2:17][N:18]3[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]3)=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.C(N(CC)CC)C.C1(C)C=CC=CC=1P(C1C=CC=CC=1C)C1C=CC=CC=1C.[C:53]([O:57][CH2:58][CH3:59])(=[O:56])[CH:54]=[CH2:55]>C(#N)C.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[CH2:58]([O:57][C:53]([CH:54]=[CH:55][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][C:11]([O:14][CH2:15][CH2:16][CH2:17][N:18]3[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]3)=[CH:10][CH:9]=2)=[CH:4][CH:3]=1)=[O:56])[CH3:59]Komponenten
7
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Versuchsvorschrift
A degazed solution of 1-{3-[(4′-bromobiphenyl-4-yl)oxy]propyl}piperidine (2.8 g), triethylamine (2.8 mL), tri(o-tolyl)phosphine (365 mg), palladium acetate (170 mg) and ethyl acrylate (2.9 mL) in acetonitrile (5 mL) is stirred at a temperature close to 60° C. for one hour, then at room temperature overnight and finally 6 h at a temperature close to 90° C. The solution is concentrated under reduced pressure, redissolved in dichloromethane, filtered and chromatographied over silica gel to give 1.3 g of 1-(3-{[4′-(2-ethoxycarbonylethen-1-yl)biphenyl-4-yl]oxy}propyl)piperidine.
Aufarbeitung
- customclose to 60° C. for one hour
- customat room temperature overnight and finally 6 h at a temperature close to 90° C
- concentrationThe solution is concentrated under reduced pressure
- dissolutionredissolved in dichloromethane
- filtrationfiltered
Quellen und Nachweise
- ORD-Eintrag
- ord-a5caf81d8889465cb3341f48ea648ec3
- Quelldatensatz
- uspto-grants-2011_12
- Patentnummer
- US08076329B2
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