Water → HCID 131716563, Verbindung

HRID 2248410Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2248410
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][C:9]2[CH:14]=[CH:13][N:12]=[CH:11][CH:10]=2)=[CH:4][CH:3]=1.[C:15](=[O:18])([O-:17])[O-:16].[K+].[K+].Cl[CH2:22][CH2:23][CH2:24][N:25]([CH2:30][CH2:31][CH2:32][CH3:33])[CH2:26][CH2:27][CH2:28][CH3:29].[OH2:34]>CS(C)=O>[C:2]([OH:1])(=[O:34])[C:15]([OH:17])=[O:18].[C:15]([OH:16])(=[O:18])[C:2]([OH:1])=[O:34].[CH2:30]([N:25]([CH2:26][CH2:27][CH2:28][CH3:29])[CH2:24][CH2:23][CH2:22][O:1][C:2]1[CH:3]=[CH:4][C:5]([S:8][C:9]2[CH:14]=[CH:13][N:12]=[CH:11][CH:10]=2)=[CH:6][CH:7]=1)[CH2:31][CH2:32][CH3:33]

Komponenten

6

Edukt 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 96084N-(3-Chloropropyl)dibutylamineHCID 150806694-(pyridin-4-ylsulfanyl)phenol

Produkt 1

HCID 131716563HCID 131716563, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 679Dimethyl SulfoxideLösungsmittel

Versuchsvorschrift

A solution of 0.014 mol of 4-(4-hydroxy-phenylthio)pyridine and 3 g of finely crushed anhydrous potassium carbonate in 50 ml of dimethylsulphoxide was placed under stirring for 30 min. To this medium 0.016 mol of 1-chloro-3-(di-n-butylamino)propane was added and the stirring was maintained at room-temperature for 24 hours. The reaction medium was poured into water and extracted with ethyl ether. The organic phase was washed with water, dried on sodium sulphate and filtered. After the solvent was evaporated off, an oil was provided which was purified by chromatography on a silica column (eluent:methanol). The required compound in free base form so obtained was then transformed into an oxalate by adding an ethereal solution of oxalic acid.

Aufarbeitung

  1. temperaturethe stirring was maintained at room-temperature for 24 hours
  2. extractionextracted with ethyl ether
  3. washThe organic phase was washed with water
  4. customdried on sodium sulphate
  5. filtrationfiltered
  6. customAfter the solvent was evaporated off
  7. customan oil was provided which
  8. customwas purified by chromatography on a silica column (eluent:methanol)

Quellen und Nachweise

ORD-Eintrag
ord-f064c40c7ddc4526bb00d938568c5a1d
Quelldatensatz
uspto-grants-1991_08
Patentnummer
US05039700

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