Hydrazine hydrate (1:1) → 4-Azafluorene

HRID 578603

Reaktionsgleichung

Reaktionsgleichung von HRID 578603
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]2[C:7](=O)[C:8]3[C:13]([C:2]=12)=[CH:12][CH:11]=[CH:10][CH:9]=3.O.NN>C(O)COCCO>[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]2[CH2:7][C:8]3[C:13]([C:2]=12)=[CH:12][CH:11]=[CH:10][CH:9]=3

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 774895H-Indeno(1,2-b)pyridin-5-one

Produkt 1

HCID 92054-AzafluoreneAusbeute 81 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8117Diethylene GlycolLösungsmittel

Reaktionsbedingungen

Temperatur
170 °C

Versuchsvorschrift

A mixture of 18.1 g (100 mmol) of 5H-indeno[1,2-b]pyridin-5-one, 27 ml (400 mmol) of hydrazine monohydrate, and 500 ml diethylene glycol was degassed and placed under nitrogen, and then heated at 170° C. for 12 h. After the reaction finish, the mixture was allowed to cool to room temperature. The organic layer was extracted with ethyl acetate and water, dried with anhydrous magnesium sulfate, the solvent was removed to give product 13.5 g (81%).

Aufarbeitung

  1. customwas degassed
  2. temperatureto cool to room temperature
  3. extractionThe organic layer was extracted with ethyl acetate and water
  4. dry with materialdried with anhydrous magnesium sulfate
  5. customthe solvent was removed

Quellen und Nachweise

ORD-Eintrag
ord-9485400a145141718cd19b05d8275b9d
Quelldatensatz
uspto-grants-2015_05
Patentnummer
US09040174B2

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