Hydrochloric Acid → 2-{2-[2-(2-Phenylethyl)phenoxy]ethyl}piperidine hydrochloride
Reaction equation
[ClH:1].C(OC([N:9]1[CH2:14][CH2:13][CH2:12][CH2:11][CH:10]1[CH2:15][CH2:16][O:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=1[CH2:24][CH2:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)=O)(C)(C)C>O1CCOCC1>[ClH:1].[C:26]1([CH2:25][CH2:24][C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=2[O:17][CH2:16][CH2:15][CH:10]2[CH2:11][CH2:12][CH2:13][CH2:14][NH:9]2)[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=1Participants
Procedure
5 ml of a 4N solution of hydrogen chloride in dioxane were added to a solution of 440 mg of 1-t-butoxycarbonyl-2-{2-[2-(2-phenylethyl)phenoxy]ethyl}piperidine [prepared as described in step (a) above] in 5 ml of dioxane, and the resulting mixture was allowed to stand at room temperature for 2 hours. At the end of this time, the solvent was removed by distillation under reduced pressure, and the resulting solid residue was dissolved in a small amount of methylene chloride; 20 ml of ethyl acetate was then added to the solution thus obtained, after which it was allowed to stand at room temperature. The crystals which precipitated were collected by filtration, to give 214 mg (yield 53%) of the title compound as colorless crystals, melting at 95°-97° C.
Workup
- customAt the end of this time, the solvent was removed by distillation under reduced pressure
- dissolutionthe resulting solid residue was dissolved in a small amount of methylene chloride
- addition20 ml of ethyl acetate was then added to the solution
- customthus obtained
- customto stand at room temperature
- customThe crystals which precipitated
- filtrationwere collected by filtration
Sources & evidence
- ORD record
- ord-9c0b8e648fec434397aec6ee17ab1fa5
- Source dataset
- uspto-grants-1996_09
- Patent number
- US05556864
Reaction notes
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