Hydrochloric Acid → HCID 67669793, compound

HRID 743356Notes

Reaction equation

HRID 743356 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 54330194HCID 54330194, compound

Product 1

HCID 67669793HCID 67669793, compoundYield 61%

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent2×

Procedure

0.800 g of (R)-4-methyl-2-[2-(2-phenylethyl)phenoxymethyl]morpholine [prepared as described in step (a) above] was dissolved in 10 ml of dioxane, and 0.8 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. The resulting oil was dissolved in 15 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 0.541 g (yield 61%) of the title compound as colorless crystals, melting at 123°-125° C.

Workup

  1. concentrationThe mixture was then concentrated by distillation under reduced pressure
  2. dissolutionThe resulting oil was dissolved in 15 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-27fa51781e0b41f19d734cc284d96d25
Source dataset
uspto-grants-1996_09
Patent number
US05556864

Reaction notes

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