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Hydrochloric Acid → 3-{2-[2-(3-Methoxyphenyl)ethyl]phenoxymethyl}-1-methylpiperidine hydrochloride

HRID 743269
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 743269
[ClH:1].[CH3:2][O:3][C:4]1[CH:5]=[C:6]([CH2:10][CH2:11][C:12]2[CH:26]=[CH:25][CH:24]=[CH:23][C:13]=2[O:14][CH2:15][CH:16]2[CH2:21][CH2:20][CH2:19][N:18]([CH3:22])[CH2:17]2)[CH:7]=[CH:8][CH:9]=1.C(OCC)(=O)C>O1CCOCC1>[ClH:1].[CH3:2][O:3][C:4]1[CH:5]=[C:6]([CH2:10][CH2:11][C:12]2[CH:26]=[CH:25][CH:24]=[CH:23][C:13]=2[O:14][CH2:15][CH:16]2[CH2:21][CH2:20][CH2:19][N:18]([CH3:22])[CH2:17]2)[CH:7]=[CH:8][CH:9]=1
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Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 100885823-{2-[2-(3-Methoxyphenyl)ethyl]phenoxymethyl}-1-methylpiperidine

Produkt 1

HCID 574976253-{2-[2-(3-Methoxyphenyl)ethyl]phenoxymethyl}-1-methylpiperidine hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

0.5 ml of a 4N solution of hydrogen chloride in dioxane was added to a solution of 520 mg of 3-{2-[2-(3-methoxyphenyl)ethyl]phenoxymethyl}-1-methylpiperidine [prepared as described in step (a) above] in a suitable amount of ethyl acetate, and the resulting mixture was concentrated by distillation under reduced pressure, to produce the hydrochloride as a solid. This solid was dissolved in a small amount of methylene chloride, and then ethyl acetate was added to the resulting solution, which was then allowed to stand at room temperature. The crystals which precipitated were collected by filtration, to give 443 mg (yield 77%) of the title compound as colorless crystals, melting at 191°-193° C.

Aufarbeitung

  1. concentrationthe resulting mixture was concentrated by distillation under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-e7d8cb4f4c394f7390d52aac95a4a302
Quelldatensatz
uspto-grants-1996_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05556864

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