Sodium Chloride → 4-Azafluorene

HRID 1093030

Reaktionsgleichung

Reaktionsgleichung von HRID 1093030
[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[N:4]=[CH:3][CH:2]=1.O.NN.[Cl-].[Na+]>C(O)COCCO>[CH:1]1[C:13]2[CH2:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[N:4]=[CH:3][CH:2]=1

Komponenten

5

Edukt 3

HCID 5234Sodium ChlorideHCID 24654Hydrazine hydrate (1:1)HCID 774895H-Indeno(1,2-b)pyridin-5-one

Produkt 1

HCID 92054-AzafluoreneAusbeute 99 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8117Diethylene GlycolLösungsmittel

Reaktionsbedingungen

Temperatur
168 °C

Versuchsvorschrift

Subsequently, in a stream of argon, 500 mL of diethylene glycol was added to 16.8 g (92.6 mmol) of 4-azafluorene-9-one and 25 mL (370 mmol) of hydrazine monohydrate, and was heated and stirred at 168° C. for 3 hours. After the reaction liquid was cooled to room temperature, an aqueous solution of sodium chloride was added to the reaction liquid, and then, was extracted with ethyl acetate. The organic phase was washed with water, dried over sodium sulfate and concentrated, to thereby obtain 15.3 g of 4-azafluorene (99% yield).

Aufarbeitung

  1. temperaturewas heated
  2. customAfter the reaction liquid
  3. temperaturewas cooled to room temperature
  4. extractionwas extracted with ethyl acetate
  5. washThe organic phase was washed with water
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-e5ea128c0996488d818612d85c2ddd28
Quelldatensatz
uspto-grants-2012_03
Patentnummer
US08129899B1

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