Hydrochloric Acid → 3-{2-[4-(3-Methoxyphenyl)butyl]phenoxymethyl}-1-methylpiperidine hydrochloride
Reaction equation
[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]=1Participants
6
Reactant 3
Product 1
Reagents, catalysts & solvents 2
Procedure
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.
Workup
- concentrationconcentrated by distillation under reduced pressure
- customto give a solid
- customto stand at room temperature
- customThe crystals which precipitated
- filtrationwere collected by filtration
- customdried in vacuo
Sources & evidence
- ORD record
- ord-b067ddbaddfa41c0b09e681211c1de31
- Source dataset
- uspto-grants-1996_09
- Patent number
- US05556864
Reaction notes
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