Hydrochloric Acid → HCID 57497651, compound

HRID 743345Notes

Reaction equation

HRID 743345 reaction equation
[Cl:1][C:2]1[CH:3]=[C:4]([CH2:8][CH2:9][C:10]2[CH:24]=[CH:23][CH:22]=[CH:21][C:11]=2[O:12][CH2:13][CH2:14][CH:15]2[CH2:19][CH2:18][CH2:17][N:16]2[CH3:20])[CH:5]=[CH:6][CH:7]=1.Cl>C(OCC)(=O)C.O1CCOCC1>[ClH:1].[Cl:1][C:2]1[CH:3]=[C:4]([CH2:8][CH2:9][C:10]2[CH:24]=[CH:23][CH:22]=[CH:21][C:11]=2[O:12][CH2:13][CH2:14][CH:15]2[CH2:19][CH2:18][CH2:17][N:16]2[CH3:20])[CH:5]=[CH:6][CH:7]=1

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 10809774HCID 10809774, compound

Product 1

HCID 57497651HCID 57497651, compoundYield 127.4%

Reagents, catalysts & solvents 2

HCID 8857Ethyl AcetateSolventHCID 312751,4-DioxaneSolvent

Procedure

0.752 g of 2-(2-{2-[2-(3-chlorophenyl)ethyl]phenoxy}ethyl)-1-methylpyrrolidine [prepared as described in step (a) above] was dissolved in 15 ml of ethyl acetate, and 0.6 ml of a 4N solution of hydrogen chloride in dioxane was added to the resulting solution. The mixture was then concentrated by distillation under reduced pressure. The concentrate was dissolved in 20 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 0.530 g (yield 64%) of the title compound as colorless crystals, melting at 119°-121° C.

Workup

  1. concentrationThe mixture was then concentrated by distillation under reduced pressure
  2. dissolutionThe concentrate was dissolved in 20 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-1773205a0dd540c796637008a0e8e7d1
Source dataset
uspto-grants-1996_09
Patent number
US05556864

Reaction notes

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