Reaktion #1095077

ord-96b64a41c607495883c81ef1f8893c3b

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe organic layer is separated
  2. 2
    Waschenwashed with water and saturated aqueous solution of sodium chloride
  3. 3
    Trocknendried over anhydrous magnesium sulfate
  4. 4
    workup.DISTILLATIONthe solvent is distilled off under reduced pressure
  5. 5
    Sonstigethe residue is purified by column chromatography (eluent: chloroform:methanol=10:1)

Vorschrift

In 6 mL of N,N-dimethylformamide is dissolved 0.80 g of 5-[2-(3-chloropropyloxy)ethyl]benzo[b]-thiophene, to which are added 0.51 mL of 2-(methylamino)ethanol and 0.87 g of potassium carbonate. The mixture is stirred at 80° C. for 3 hours. The reaction mixture is introduced into a mixture of water and ethyl acetate. The organic layer is separated, washed with water and saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate, the solvent is distilled off under reduced pressure, and the residue is purified by column chromatography (eluent: chloroform:methanol=10:1). Thus, 0.59 g of 2-{[3-(2-benzo[b]thiophen-5-ylethoxy)propyl]-(methyl)amino]-1-ethanol is obtained as an oily product.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06797726B1uspto-grants-2004_09