Hydrochloric Acid → HCID 57497659, compound

HRID 743367Notes

Reaction equation

HRID 743367 reaction equation
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:11][CH2:12][C:13]2[CH:27]=[CH:26][CH:25]=[CH:24][C:14]=2[O:15][CH2:16][CH2:17][C@@H:18]2[CH2:22][CH2:21][CH2:20][N:19]2[CH3:23])[CH:6]=[C:7]([O:9][CH3:10])[CH:8]=1.[ClH:28]>O1CCOCC1>[ClH:28].[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:11][CH2:12][C:13]2[CH:27]=[CH:26][CH:25]=[CH:24][C:14]=2[O:15][CH2:16][CH2:17][C@@H:18]2[CH2:22][CH2:21][CH2:20][N:19]2[CH3:23])[CH:6]=[C:7]([O:9][CH3:10])[CH:8]=1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 54158319HCID 54158319, compound

Product 1

HCID 57497659HCID 57497659, compoundYield 60%

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent2×

Procedure

0.545 g of (S)-2-(2-{2-[2-(3,5-dimethoxyphenyl)ethyl]phenoxy}ethyl)-1-methylpyrrolidine [prepared as described in step (b) above] was dissolved in 8 ml of dioxane, and 1.11 ml of a 4N solution of hydrogen chloride in dioxane was added to the solution, which was then concentrated by distillation under reduced pressure. The resulting oil was dissolved in 10 ml of ethyl acetate, and the solution was allowed to stand at room temperature. The crystals which precipitated were collected by filtration and dried in vacuo, to give 0.361 g (yield 60%) of the title compound as colorless crystals, melting at 125°-126° C.

Workup

  1. concentrationwas 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-fba662c2e4814ab7a9b460de020abdb6
Source dataset
uspto-grants-1996_09
Patent number
US05556864

Reaction notes

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