Hydrochloric Acid → HCID 67668991, compound

HRID 743358Notes

Reaction equation

HRID 743358 reaction equation
[CH3:1][N:2]1[CH2:7][CH2:6][O:5][C@H:4]([CH2:8][O:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[CH2:16][CH2:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH2:3]1.[ClH:24]>O1CCOCC1>[ClH:24].[CH3:1][N:2]1[CH2:7][CH2:6][O:5][C@H:4]([CH2:8][O:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[CH2:16][CH2:17][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH2:3]1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 54330193HCID 54330193, compound

Product 1

HCID 67668991HCID 67668991, compoundYield 72%

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent2×

Procedure

0.560 g of (S)-4-methyl-2-[2-(2-phenylethyl)phenoxymethyl]morpholine [prepared as described in step (a) above] was dissolved in 5 ml of dioxane, and 0.56 ml of a 4N solution of hydrogen chloride in dioxane was added to the solution. The mixture was then concentrated by distillation under reduced pressure, and the resulting oil was dissolved in 10 ml of ethyl acetate and allowed to stand at room temperature. The crystals which precipitated were collected by filtration and dried in vacuo, to give 0.448 g (yield 72%) of the title compound as colorless crystals, melting at 125°-127° C.

Workup

  1. concentrationThe mixture was then concentrated by distillation under reduced pressure
  2. dissolutionthe resulting oil was dissolved in 10 ml of ethyl acetate
  3. customto stand at room temperature
  4. customThe crystals which precipitated
  5. filtrationwere collected by filtration
  6. customdried in vacuo

Sources & evidence

ORD record
ord-92cca8e679b6448290ac42668b16281e
Source dataset
uspto-grants-1996_09
Patent number
US05556864

Reaction notes

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