Reaktion #336399

ord-074674d285564107b76fd54162c85127

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGfurther stirring for 30 minutes at 85°-88° C
  2. 2
    SonstigeAfter the reaction
  3. 3
    Temperaturthe reaction mixture was cooled
  4. 4
    Sonstigeto precipitate a crystal
  5. 5
    SonstigeThe crystal was recrystallized from a mixture solvent of toluene-acetone

Vorschrift

Then, in a 50 ml-three-necked flask, 0.32 g (2.22 mM) of heptanohydrazide and 15 ml of dioxane were placed. To the mixture, a solution of the above-prepared 7-octyl-2-fluorenecarbonyl chloride in 5 ml of dioxane was added, followed by addition of 0.84 ml of pyridine at about 85° C. under stirring and further stirring for 30 minutes at 85°-88° C. After the reaction, the reaction mixture was cooled and poured into 200 ml of ice water to precipitate a crystal. The crystal was recrystallized from a mixture solvent of toluene-acetone to obtain 0.68 g of N-heptanoyl-N'-(7-octyl-2-fluorenecarbonyl) hydrazine (Yield: 69.8%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05213709uspto-grants-1993_05