Reaktion #336399
ord-074674d285564107b76fd54162c85127
Reaktionsgleichung
Reagenzien
Keine
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1workup.STIRRINGfurther stirring for 30 minutes at 85°-88° C
- 2SonstigeAfter the reaction
- 3Temperaturthe reaction mixture was cooled
- 4Sonstigeto precipitate a crystal
- 5SonstigeThe 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%).