Reaktion #5144

ord-90395268b2774bc9b14694b06a459c4d

Reaktionsgleichung

OCCOCCOCCCl
2-(2-(2-chloroethoxy)ethoxy)-ethanol
O=[N+]([O-])c1cccc(O)c1
m-nitrophenol
CN(C)C=O
N,N-dimethylformamide
O=C([O-])[O-].[K+].[K+]
potassium carbonate
O=[N+]([O-])c1cccc(OCCOCCOCCO)c1
2-(2-(2-(3-nitrophenoxy)ethoxy)ethoxy)ethanol

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGAfter stirring the mixture for one hour at 80° C.
  2. 2
    Extraktionthe ethyl acetate layer was extracted
  3. 3
    WaschenThe ethyl acetate layer was washed with 200 ml of water
  4. 4
    Einengenconcentrated
  5. 5
    Sonstigeto remove ethyl acetate

Vorschrift

While stirring a mixture of 27.8 g of m-nitrophenol, 120 ml of N,N-dimethylformamide, and 25 g of potassium carbonate at 80° C., 37 g of 2-(2-(2-chloroethoxy)ethoxy)-ethanol was added dropwise to the mixture. After stirring the mixture for one hour at 80° C., 200 ml of ethyl acetate and 200 ml of water were added to the reaction mixture and the ethyl acetate layer was extracted. The ethyl acetate layer was washed with 200 ml of water and concentrated to remove ethyl acetate to provide 2-(2-(2-(3-nitrophenoxy)ethoxy)ethoxy)ethanol (1-A).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05243004uspto-grants-1993_09