Hydrochloric Acid → 9-Fluorenone hydrazone

HRID 1241221

Reaktionsgleichung

Reaktionsgleichung von HRID 1241221
[CH:1]1[C:13]2[C:12](=O)[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1.O.[NH2:16][NH2:17].Cl>CC(O)C>[CH:1]1[C:13]2[C:12](=[N:16][NH2:17])[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 10241FluorenoneHCID 24654Hydrazine hydrate (1:1)

Produkt 1

HCID 836279-Fluorenone hydrazoneAusbeute 74 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776IsopropanolLösungsmittel

Versuchsvorschrift

9-Fluorenone (200 g, 1.1 mol, from Aldrich, Milwaukee, Wis.) and hydrazine monohydrate (160 ml, 3.3 mol, from Aldrich, Milwaukee, Wis.) were dissolved in 1000 ml of 2-propanol in a 2000 ml 2-neck round bottom flask equipped with a reflux condenser and a mechanical stirrer. Concentrated hydrochloric acid (4 ml) was then added, and the mixture was refluxed for one hour. The mixture was cooled slowly to room temperature, and the crude solid product was harvested by filtration. The solid was washed with isopropanol and then recrystallized from dioxane to obtain 150 g (74% yield) of 9-fluorenone hydrazone.

Aufarbeitung

  1. customequipped with a reflux condenser and a mechanical stirrer
  2. temperaturethe mixture was refluxed for one hour
  3. filtrationthe crude solid product was harvested by filtration
  4. washThe solid was washed with isopropanol
  5. customrecrystallized from dioxane

Quellen und Nachweise

ORD-Eintrag
ord-4e487b3cec564faea8c88468adbf93de
Quelldatensatz
uspto-grants-2006_10
Patentnummer
US07115347B2

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