Hydrochloric Acid → HCID 57497655, compound

HRID 743352Notes

Reaction equation

HRID 743352 reaction equation
[CH2:1]([O:3][C:4]1[CH:5]=[C:6]([CH2:10][CH2:11][C:12]2[CH:26]=[CH:25][CH:24]=[CH:23][C:13]=2[O:14][CH2:15][CH2:16][CH:17]2[CH2:21][CH2:20][CH2:19][N:18]2[CH3:22])[CH:7]=[CH:8][CH:9]=1)[CH3:2].[ClH:27]>C(OCC)(=O)C.O1CCOCC1>[ClH:27].[CH2:1]([O:3][C:4]1[CH:5]=[C:6]([CH2:10][CH2:11][C:12]2[CH:26]=[CH:25][CH:24]=[CH:23][C:13]=2[O:14][CH2:15][CH2:16][CH:17]2[CH2:21][CH2:20][CH2:19][N:18]2[CH3:22])[CH:7]=[CH:8][CH:9]=1)[CH3:2]

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 10834229HCID 10834229, compound

Product 1

HCID 57497655HCID 57497655, compoundYield 53%

Reagents, catalysts & solvents 2

HCID 8857Ethyl AcetateSolventHCID 312751,4-DioxaneSolvent

Procedure

0.891 g of 2-(2-{2-[2-(3-ethoxyphenyl)ethyl]phenoxy}ethyl)-1-methylpyrrolidine [prepared as described in step (a) above] was dissolved in a small amount of ethyl acetate, and 0.76 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 concentrate was dissolved in 25 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 0.518 g (yield 53%) of the title compound as colorless crystals, melting at 120°-121° C.

Workup

  1. additionwas added to the solution
  2. concentrationThe mixture was then concentrated by distillation under reduced pressure
  3. dissolutionthe concentrate was dissolved in 25 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-ce28d9cf97914d61b69afb138c6e8d68
Source dataset
uspto-grants-1996_09
Patent number
US05556864

Reaction notes

Loading…