Potassium Carbonate → 1-[N(1-phenoxy-2-propyl)piperazino]-1-phenyl acetone

HRID 1704735Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1704735
[O:1]([CH2:8][CH:9]([N:11]1[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]1)[CH3:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH:24]([C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)[C:25]([CH3:27])=[O:26]>CC(CC)=O>[O:1]([CH2:8][CH:9]([N:11]1[CH2:12][CH2:13][N:14]([CH:24]([C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)[C:25]([CH3:27])=[O:26])[CH2:15][CH2:16]1)[CH3:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Komponenten

5

Versuchsvorschrift

To N(1-phenoxy-2-propyl)piperazine (1 mole) dissolved in methylethylketone (1000 ml) are added dry potassium carbonate (2 moles) and 1-bromo-1-phenyl-acetone (1 mole). The mixture is refluxed during 5 hours, with stirring. The solvent is evaporated off in vacuo. The residue is taken up into water and is then extracted with methylene chloride. The organic phase is washed with water to neutral pH. The organic phase is extracted with a dilute aqueous hydrochloric acid solution and is then concentrated in vacuo, over a water-bath. The resulting oil is taken up into boiling 95% ethyl alcohol, to give, on cooling, white crystals, M.p. 177°-180° C. N.M.R.: consistent.

Aufarbeitung

  1. temperatureThe mixture is refluxed during 5 hours
  2. customThe solvent is evaporated off in vacuo
  3. extractionis then extracted with methylene chloride
  4. washThe organic phase is washed with water to neutral pH
  5. extractionThe organic phase is extracted with a dilute aqueous hydrochloric acid solution
  6. concentrationis then concentrated in vacuo, over a water-bath
  7. customto give
  8. temperatureon cooling

Quellen und Nachweise

ORD-Eintrag
ord-35c55519e1c94edea0c4b603d9302285
Quelldatensatz
uspto-grants-1978_11
Patentnummer
US04127661

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