Hydrochloric Acid → HCID 57497619, compound
Reaction equation
[ClH:1].C(OC([N:9]1[CH2:14][CH2:13][O:12][C@@H:11]([CH2:15][O:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=2[CH2:23][CH2:24][C:25]2[CH:30]=[CH:29][CH:28]=[C:27]([O:31][CH3:32])[CH:26]=2)[CH2:10]1)=O)(C)(C)C>O1CCOCC1>[ClH:1].[CH3:32][O:31][C:27]1[CH:26]=[C:25]([CH2:24][CH2:23][C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=2[O:16][CH2:15][C@@H:11]2[O:12][CH2:13][CH2:14][NH:9][CH2:10]2)[CH:30]=[CH:29][CH:28]=1Participants
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
10 ml of a 4N solution of hydrogen chloride in dioxane were added to a solution of 1.68 g of (R)-4-t-butoxycarbonyl-2-{2-[2-(3-methoxyphenyl)ethyl]phenoxymethyl}morpholine [prepared as described in step (a) above] in 10 ml of dioxane, and the resulting mixture 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 residue was dissolved in a small amount of methylene chloride. Ethyl acetate was added to the mixture, which was then allowed to stand at room temperature. The crystals which precipitated were collected by filtration and dried in vacuo, to give 1.24 g (yield 86%) of the title compound as colorless crystals, melting at 112°-113° C.
Workup
- customAt the end of this time, the solvent was removed by distillation under reduced pressure
- dissolutionthe resulting residue was dissolved in a small amount of methylene chloride
- additionEthyl acetate was added to the mixture, which
- customto stand at room temperature
- customThe crystals which precipitated
- filtrationwere collected by filtration
- customdried in vacuo
Sources & evidence
- ORD record
- ord-240c4f8ff414467eb2d05ce5f6aac50c
- Source dataset
- uspto-grants-1996_09
- Patent number
- US05556864
Reaction notes
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