Water → 3-(2-Tetrahydropyranyloxyethyl)-3-(3,4-dichlorophenyl)piperidine

HRID 1080661Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1080661
[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]1

Komponenten

6

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

  1. temperatureThe reaction mixture is heated for one hour at 60° C.
  2. temperaturecooled
  3. filtrationThe insoluble portion is filtered off
  4. concentrationthe filtrate is concentrated under vacuum
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-4675d69f721c44bbbd5d7b486d41ffbb
Quelldatensatz
uspto-grants-1996_12
Patentnummer
US05583134

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