Methanol → HCID 9975721, Verbindung

HRID 487137

Reaktionsgleichung

[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:23]2[CH:28]=[CH:27][C:26]([F:29])=[CH:25][CH:24]=2)[O:9][CH2:10][CH2:11][N:12]2[CH2:17][CH2:16][CH:15]([C:18](OCC)=[O:19])[CH2:14][CH2:13]2)=[CH:4][CH:3]=1.[H-].C([Al+]CC(C)C)C(C)C.CO.[Cl-].[NH4+]>C1(C)C=CC=CC=1.CCCCCC>[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:23]2[CH:28]=[CH:27][C:26]([F:29])=[CH:25][CH:24]=2)[O:9][CH2:10][CH2:11][N:12]2[CH2:17][CH2:16][CH:15]([CH:18]=[O:19])[CH2:14][CH2:13]2)=[CH:4][CH:3]=1

Komponenten

Reaktionsbedingungen

Temperatur: -68 °C

Versuchsvorschrift

3.03 g of ethyl 1-[2-bis(4-fluorophenyl)methoxyethyl]-4-piperidinecarboxylate (prepared as described in preparation 8) were dissolved in 30 ml of toluene, under a stream of nitrogen, and the resulting solution was cooled at -68° C. 8.2 ml of a 1M solution of diisobutylaluminum hydride in hexane was then added dropwise to the cooled mixture over a period of 10 minutes, and the mixture was stirred for 1 hour at -68° C. At the end of this time, 2 ml of methanol and 3 ml of a saturated aqueous solution of ammonium chloride were added to the reaction solution. The mixture was then extracted with ethyl acetate, to give 2.47 g (yield 91%) of the title compound as an oil, whose properties were the same as those of the product of step (a).

Aufarbeitung

extractionThe mixture was then extracted with ethyl acetate

Quellen und Nachweise

ORD-Eintrag: ord-cbe09b54350b4e8787548fce94d652ef
Quelldatensatz: uspto-grants-1994_03
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US05294623

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