Hydrochloric Acid → HCID 57497654, compound

HRID 743348Notes

Reaction equation

HRID 743348 reaction equation
[F: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.[ClH:25]>C(OCC)(=O)C.O1CCOCC1>[ClH:25].[F: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 10761245HCID 10761245, compound

Product 1

HCID 57497654HCID 57497654, compoundYield 56%

Reagents, catalysts & solvents 2

HCID 8857Ethyl AcetateSolventHCID 312751,4-DioxaneSolvent

Procedure

0.923 g of 2-(2-{2-[2-(3-fluorophenyl)ethyl]phenoxy}ethyl)-1-methylpyrrolidine [prepared as described in step (a) above] was dissolved in 15 ml of ethyl acetate, 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 concentrate was dissolved in 25 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 0.585 g (yield 56%) of the title compound as colorless crystals, melting at 135°-136° C.

Workup

  1. concentrationThe mixture was then concentrated by distillation under reduced pressure
  2. dissolutionThe concentrate was dissolved in 25 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-a7aef63cab604c56826867564467db41
Source dataset
uspto-grants-1996_09
Patent number
US05556864

Reaction notes

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