Hydrochloric Acid → HCID 19423876, compound

HRID 743377Notes

Reaction equation

HRID 743377 reaction equation
[F:1][CH:2]([F:27])[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][CH:16]2[CH2:21][CH2:20][CH2:19][N:18]([CH3:22])[CH2:17]2)[CH:7]=[CH:8][CH:9]=1.[ClH:28]>O1CCOCC1>[ClH:28].[F:27][CH:2]([F: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][CH:16]2[CH2:21][CH2:20][CH2:19][N:18]([CH3:22])[CH2:17]2)[CH:7]=[CH:8][CH:9]=1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 19423877HCID 19423877, compound

Product 1

HCID 19423876HCID 19423876, compoundYield 70%

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent2×

Procedure

0.56 g of 3-{2-[2-(3-difluoromethoxyphenyl)ethyl]phenoxymethyl}-1-methylpiperidine [prepared as described in step (a) above] was dissolved in 5 ml of dioxane, and 0.45 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 solid was dissolved in a small amount of methanol, and about 50 ml of ethyl acetate were added to the solution, which was then allowed to stand at room temperature for one hour. The crystals which precipitated were collected by filtration and dried in vacuo, to give 0.43 g (yield 70%) of the title compound as colorless crystals, melting at 174°-175° C.

Workup

  1. concentrationwas then concentrated by distillation under reduced pressure
  2. dissolutionThe resulting solid was dissolved in a small amount of methanol, and about 50 ml of ethyl acetate
  3. additionwere added to the solution, which
  4. customThe crystals which precipitated
  5. filtrationwere collected by filtration
  6. customdried in vacuo

Sources & evidence

ORD record
ord-985e946dc9b144e3ac8d2ee33673b751
Source dataset
uspto-grants-1996_09
Patent number
US05556864

Reaction notes

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