Reaktion #433174

ord-321ec6453f6d406e908ab288eb00b8ed

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter cooling
  2. 2
    Extraktionthe mixture is extracted three times
  3. 3
    WaschenThe CH2Cl2 solution is washed with water
  4. 4
    Trocknendried over Na2SO4
  5. 5
    Sonstigeevaporated
  6. 6
    workup.DISSOLUTIONThe oily residue is dissolved in hexane/acetone
  7. 7
    Sonstigepurified chromatographically on an SiO2 column

Vorschrift

15 g (36.4 mmol) of the product from Example 18 are heated to 120° for 3 hours together with 30 ml of octylamine. After cooling, 40 ml of water are added and the mixture is extracted three times using 30 ml of methylene chloride. The CH2Cl2 solution is washed with water, dried over Na2SO4 and evaporated. The oily residue is dissolved in hexane/acetone and purified chromatographically on an SiO2 column. The main fraction is a viscous material.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05059689uspto-grants-1991_10