Reaktion #2069926

ord-8826973177f346569a29a8230f5bbb3c

Reaktionsgleichung

CC(=O)N(c1ccc(C(C)C)cc1)c1ccc(C(C)C)cc1
N-Acetyl-N,N-di(4-isopropylphenyl)amine
CC(C)c1ccc(Nc2ccc(C(C)C)cc2)cc1
N,N-Di-(4-isopropylphenyl)amine

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONThe ethanolic solution is poured into dist
  2. 2
    Filtrationwater, and the brownish precipitate is filtered off with suction
  3. 3
    workup.DISSOLUTIONdissolved in dichloromethane
  4. 4
    Trocknendried with sodium sulphate
  5. 5
    EinengenThe solution is concentrated
  6. 6
    Sonstigechromatographed through a short silica gel column with 50% dichloromethane in hexane
  7. 7
    EinengenThe product fractions are concentrated to dryness
  8. 8
    Sonstigethe product is dried under reduced pressure

Vorschrift

N-Acetyl-N,N-di(4-isopropylphenyl)amine (5.4 g, 18.4 mmol) are heated to reflux in 100 ml of 20% aqueous ethanol. The reaction is monitored by thin-layer chromatography. After 30 h, no reactant is any longer detectable in the TLC. The ethanolic solution is poured into dist. water, and the brownish precipitate is filtered off with suction, dissolved in dichloromethane and dried with sodium sulphate. The solution is concentrated and chromatographed through a short silica gel column with 50% dichloromethane in hexane. The product fractions are concentrated to dryness and the product is dried under reduced pressure.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07540978B2uspto-grants-2009_06