Reaktion #49803

ord-747da01c1a934f2ca7eb9695b5039c16

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted with ether
  2. 2
    WaschenThe combined organic extracts are washed sequentially with one molar hydrochloric acid, water and brine
  3. 3
    Trocknendried over anhydrous magnesium sulfate
  4. 4
    Einengenconcentrated in vacuo
  5. 5
    Sonstigeto obtain an oil

Vorschrift

Benzyl alcohol (0.8 mL, 7.73 mmol) and triethylamine (1 mL, 7.17 mmol) are added to a mixture of {o-[5-(2,4-dichlorophenoxy)-2-nitrophenoxy]phenoxy}acetyl chloride (1.12 g, 2.38 mmol) in tetrahydrofuran. The reaction mixture is stirred for twenty minutes, poured into water and extracted with ether. The combined organic extracts are washed sequentially with one molar hydrochloric acid, water and brine, dried over anhydrous magnesium sulfate and concentrated in vacuo to obtain an oil. Column chromatography of the oil using silica gel and a hexanes in methylene chloride solution gives the title product as a yellow oil (1.0 g) which is identified by NMR spectral analyses.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05424280uspto-grants-1995_06