Water → 3-(2-Tetrahydropyranyloxyethyl)-3-(3,4-dichlorophenyl)piperidine
Reaktionsgleichung
[O:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]1[O:7][CH2:8][CH2:9][C:10]1([C:17]2[CH:22]=[CH:21][C:20]([Cl:23])=[C:19]([Cl:24])[CH:18]=2)[CH2:15][NH:14][C:13](=O)[CH2:12][CH2:11]1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1>[O:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]1[O:7][CH2:8][CH2:9][C:10]1([C:17]2[CH:22]=[CH:21][C:20]([Cl:23])=[C:19]([Cl:24])[CH:18]=2)[CH2:11][CH2:12][CH2:13][NH:14][CH2:15]1Komponenten
6
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 60 °C
Versuchsvorschrift
3.9 g of the 5-(2-tetrahydropyranyloxyethyl)-5-(3,4-dichlorophenyl)piperidinone prepared above are dissolved in 50 ml of tetrahydrofuran and the solution is added to a suspension of 0.9 g of lithium aluminum hydride in 5 ml of THF heated to 60° C. The reaction mixture is heated for one hour at 60° C. and then cooled. 1 ml of water, 1 ml of 4N sodium hydroxide and 3 ml of water are added. The insoluble portion is filtered off and the filtrate is concentrated under vacuum. The residue is taken up in ethyl ether, dried over MgSO4 and concentrated under vacuum to give 3.4 g of the expected product.
Aufarbeitung
- temperatureThe reaction mixture is heated for one hour at 60° C.
- temperaturecooled
- filtrationThe insoluble portion is filtered off
- concentrationthe filtrate is concentrated under vacuum
- dry with materialdried over MgSO4
- concentrationconcentrated under vacuum
Quellen und Nachweise
- ORD-Eintrag
- ord-4acb0966519f4976bf2a250e1e068580
- Quelldatensatz
- uspto-grants-1998_01
- Patentnummer
- US05712288
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