Hydrochloric Acid → 2-[2-(4-Phenylbutyl)phenoxymethyl]morpholine hydrochloride
Reaction equation
C(OC([N:8]1[CH2:13][CH2:12][O:11][CH:10]([CH2:14][O:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[CH2:22][CH2:23][CH2:24][CH2:25][C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[CH2:9]1)=O)(C)(C)C.[ClH:32]>O1CCOCC1>[ClH:32].[C:26]1([CH2:25][CH2:24][CH2:23][CH2:22][C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=2[O:15][CH2:14][CH:10]2[O:11][CH2:12][CH2:13][NH:8][CH2:9]2)[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1Participants
4
Procedure
671 mg of 4-t-butoxycarbonyl-2-[2-(4-phenylbutyl)phenoxymethyl]morpholine [prepared as described in step (a) above] was dissolved in 10 ml of a 4N solution of hydrogen chloride in dioxane, whilst ice-cooling, and the resulting solution was allowed to stand at room temperature for 30 minutes. At the end of this time, the solvent was removed by distillation under reduced pressure, and the resulting oily residue was dissolved in 20 ml of ethyl acetate. The solution thus obtained was then allowed to stand at room temperature. The crystals which precipitated were collected by filtration and dried in vacuo, to give 494 mg (yield 86%) of the title compound as colorless crystals, melting at 131°-132° C.
Workup
- temperaturecooling
- customAt the end of this time, the solvent was removed by distillation under reduced pressure
- dissolutionthe resulting oily residue was dissolved in 20 ml of ethyl acetate
- customThe solution thus obtained
- customto stand at room temperature
- customThe crystals which precipitated
- filtrationwere collected by filtration
- customdried in vacuo
Sources & evidence
- ORD record
- ord-5d2dbb9ec4da44e5bf0a3741e7e0f4d6
- Source dataset
- uspto-grants-1996_09
- Patent number
- US05556864
Reaction notes
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