Potassium Carbonate → 2-[3-(4-Phenylpiperazin-1-yl)propylthio]benzylalcohol

HRID 1789371Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1789371
[OH:1][CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[SH:9].Cl.Cl.Cl[CH2:13][CH2:14][CH2:15][N:16]1[CH2:21][CH2:20][N:19]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[CH2:18][CH2:17]1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[C:22]1([N:19]2[CH2:18][CH2:17][N:16]([CH2:15][CH2:14][CH2:13][S:9][C:4]3[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=3[CH2:2][OH:1])[CH2:21][CH2:20]2)[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 1382782-MercaptobenzenemethanolHCID 123996821-(3-Chloropropyl)-4-phenylpiperazine dihydrochloride

Produkt 1

HCID 137680822-[3-(4-Phenylpiperazin-1-yl)propylthio]benzylalcoholAusbeute 91 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

A mixture of 1.56 g of 2-(hydroxymethyl)thiophenol, 3.77 g of 1-(3-chloropropyl)-4-phenylpiperazine dihydrochloride, 5.02 g of potassium carbonate and 40 ml of dimethylformamide is stirred at 50° C. for 6 hours. Insoluble materials are filtered off, and the filtrate is concentrated under reduced pressure to remove solvent. Water is added to the residue, and the aqueous mixture is extracted with ethyl acetate. The extract is washed with water, dried and concentrated under reduced pressure to remove solvent. The residue is digested with n-hexane and collected by filtration. 3.42 g of 2-[3-(4-phenylpiperazin-1-yl)propylthio]benzylalcohol are obtained. Yield: 91%.

Aufarbeitung

  1. filtrationInsoluble materials are filtered off
  2. concentrationthe filtrate is concentrated under reduced pressure
  3. customto remove solvent
  4. additionWater is added to the residue
  5. extractionthe aqueous mixture is extracted with ethyl acetate
  6. washThe extract is washed with water
  7. customdried
  8. concentrationconcentrated under reduced pressure
  9. customto remove solvent
  10. filtrationcollected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-55e7ad6b22ff44e29d699b8a2b766ad4
Quelldatensatz
uspto-grants-1987_08
Patentnummer
US04689327

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