Hydrochloric Acid → HCID 57497657, compound

HRID 743359Notes

Reaction equation

HRID 743359 reaction equation
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH2:10][C:11]2[CH:25]=[CH:24][CH:23]=[CH:22][C:12]=2[O:13][CH2:14][CH2:15][CH:16]2[CH2:20][CH2:19][CH2:18][N:17]2[CH3:21])=[CH:5][CH:4]=1.[ClH:26]>O1CCOCC1>[ClH:26].[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([CH2:9][CH2:10][C:11]2[CH:25]=[CH:24][CH:23]=[CH:22][C:12]=2[O:13][CH2:14][CH2:15][CH:16]2[CH2:20][CH2:19][CH2:18][N:17]2[CH3:21])=[CH:7][CH:8]=1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 10547504HCID 10547504, compound

Product 1

HCID 57497657HCID 57497657, compoundYield 50%

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent2×

Procedure

0.602 g of 2-(2-{2-[2-(4-methoxyphenyl)ethyl]phenoxy}ethyl)-1-methylpyrrolidine [prepared as described in step (a) above] was dissolved in a small amount of dioxane, and 0.66 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 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 0.331 g (yield 50%) of the title compound as colorless crystals, melting at 136°-138° C.

Workup

  1. additionwas added to the solution
  2. concentrationThe mixture was then concentrated by distillation under reduced pressure
  3. dissolutionthe resulting oil was dissolved in 15 ml of ethyl acetate
  4. customto stand at room temperature
  5. customThe crystals which precipitated
  6. filtrationwere collected by filtration
  7. customdried in vacuo

Sources & evidence

ORD record
ord-deb9dd713d274b0a871d30bf59a9c55f
Source dataset
uspto-grants-1996_09
Patent number
US05556864

Reaction notes

Loading…