Hydrochloric Acid → 3-{2-[4-(3-Methoxyphenyl)butyl]phenoxymethyl}-1-methylpiperidine hydrochloride

HRID 743330Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 743330
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:9][CH2:10][CH2:11][CH2:12][C:13]2[CH:27]=[CH:26][CH:25]=[CH:24][C:14]=2[O:15][CH2:16][CH:17]2[CH2:22][CH2:21][CH2:20][N:19]([CH3:23])[CH2:18]2)[CH:6]=[CH:7][CH:8]=1.[ClH:28].C(OCC)(=O)C>O1CCOCC1.CO>[ClH:28].[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:9][CH2:10][CH2:11][CH2:12][C:13]2[CH:27]=[CH:26][CH:25]=[CH:24][C:14]=2[O:15][CH2:16][CH:17]2[CH2:22][CH2:21][CH2:20][N:19]([CH3:23])[CH2:18]2)[CH:6]=[CH:7][CH:8]=1

Komponenten

6

Versuchsvorschrift

2.10 g of 3-{2-[4-(3-methoxyphenyl)butyl]phenoxymethyl}-1-methylpiperidine [prepared as described in step (a) above] were dissolved in 10 ml of dioxane, and 1.7 ml of a 4N solution of hydrogen chloride in dioxane was added to the solution, which was shaken and then concentrated by distillation under reduced pressure to give a solid. The solid was dissolved in a small amount of methanol, and then 50 ml of ethyl acetate were added to the solution. The resulting mixture was then allowed to stand at room temperature. The crystals which precipitated were collected by filtration and dried in vacuo, to give 1.92 g (yield 83%) of the title compound as colorless needles, melting at 141°-142.5° C.

Aufarbeitung

  1. concentrationconcentrated by distillation under reduced pressure
  2. customto give a solid
  3. customto stand at room temperature
  4. customThe crystals which precipitated
  5. filtrationwere collected by filtration
  6. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-b067ddbaddfa41c0b09e681211c1de31
Quelldatensatz
uspto-grants-1996_09
Patentnummer
US05556864

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