Réaction #2069926

ord-8826973177f346569a29a8230f5bbb3c

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  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
    Séchagedried with sodium sulphate
  5. 5
    ConcentrationThe solution is concentrated
  6. 6
    Autrechromatographed through a short silica gel column with 50% dichloromethane in hexane
  7. 7
    ConcentrationThe product fractions are concentrated to dryness
  8. 8
    Autrethe product is dried under reduced pressure

Mode opératoire

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.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US07540978B2uspto-grants-2009_06