Water → 1-Azaphenanthrene-5,6-dione

HRID 1093028

Reaktionsgleichung

Reaktionsgleichung von HRID 1093028
[N:1]1[C:14]2[CH:13]=[CH:12][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:15]=I(OI(=O)=O)=O.[OH2:22]>C(O)(=O)C>[N:1]1[C:14]2[C:5](=[C:6]3[C:11](=[CH:12][CH:13]=2)[CH:10]=[CH:9][C:8](=[O:22])[C:7]3=[O:15])[CH:4]=[CH:3][CH:2]=1

Komponenten

5

Edukt 3

HCID 962WaterHCID 6796Benzo(F)QuinolineHCID 159402Iodine pentoxide

Produkt 1

HCID 199224561-Azaphenanthrene-5,6-dioneAusbeute 68 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
108 °C

Versuchsvorschrift

A solution of 68.3 g (381 mmol) of 1-azaphenanthrene and 157 g (470 mmol) of iodopentoxide in acetic acid was stirred under heat at 108° C. for 2 hours. After the reaction liquid had been cooled to room temperature, water was added to the reaction liquid to crystallize the product, and then the crystals were filtered off. Subsequently, the resultant crystal was dissolved in chloroform, washed with an aqueous solution of sodium hydrogen carbonate and an aqueous solution of sodium thiosulfate, dried, and exsiccated by concentration, whereby 53.9 g of 1-azaphenanthrene-5,6-dione were obtained (68% yield).

Aufarbeitung

  1. customAfter the reaction liquid
  2. temperaturehad been cooled to room temperature
  3. customto crystallize the product
  4. filtrationthe crystals were filtered off
  5. dissolutionSubsequently, the resultant crystal was dissolved in chloroform
  6. washwashed with an aqueous solution of sodium hydrogen carbonate
  7. dry with materialan aqueous solution of sodium thiosulfate, dried
  8. concentrationexsiccated by concentration

Quellen und Nachweise

ORD-Eintrag
ord-f91c9b8f1e2b4b9aa6a9bb83f4cdf4ba
Quelldatensatz
uspto-grants-2012_03
Patentnummer
US08129899B1

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