Reaktion #1674385

ord-b0b86372d756477d9cfc48622dbf0d6f

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionthe reaction mixture was extracted twice with 100 ml and 50 ml of chloroform
  2. 2
    Waschenthe extract was washed with a saturated sodium chloride aqueous solution
  3. 3
    Trocknendried over magnesium sulfate
  4. 4
    Sonstigeevaporated
  5. 5
    Sonstigeto remove the solvent under a reduced pressure
  6. 6
    Wascheneluted with chloroform

Vorschrift

3.24 g of ortho-phenylenediamine was dissolved in 30 ml of dimithylformaide, to the solution were added 2.07 g of potassium carbonate and 1.52 g of cinnamyl chloride, and the mixture was stirred overnight at a room temperature. After adding 100 ml of water, the reaction mixture was extracted twice with 100 ml and 50 ml of chloroform, and the extract was washed with a saturated sodium chloride aqueous solution, dried over magnesium sulfate and evaporated to remove the solvent under a reduced pressure. The resulting residue was applied to a silica gel column and eluted with chloroform, to obtain 2.0 g of the title compound as light brown crystals.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05216150uspto-grants-1993_06