9,10-Phenanthrenedione → 10-(3,5-Dichloro-2-pyridylazo)-9-phenanthrol

HRID 1266920

Reaktionsgleichung

Reaktionsgleichung von HRID 1266920
[CH:1]1[C:14]2[C:13](=O)[C:12](=[O:16])[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1.[Cl:17][C:18]1[C:19]([NH:25][NH2:26])=[N:20][CH:21]=[C:22]([Cl:24])[CH:23]=1>C(O)(=O)C>[Cl:17][C:18]1[C:19]([N:25]=[N:26][C:13]2[C:14]3[CH:1]=[CH:2][CH:3]=[CH:4][C:5]=3[C:6]3[C:11](=[CH:10][CH:9]=[CH:8][CH:7]=3)[C:12]=2[OH:16])=[N:20][CH:21]=[C:22]([Cl:24])[CH:23]=1

Komponenten

4

Edukt 2

HCID 67639,10-Phenanthrenedione2×HCID 6009663,5-Dichloro-2-hydrazinylpyridine

Produkt 1

HCID 13571850810-(3,5-Dichloro-2-pyridylazo)-9-phenanthrol

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
105 °C

Versuchsvorschrift

Next, a reaction flask was loaded with acetic acid (15 ml) and 9,10-phenanthrenequinone (5.0 g), and the temperature was raised to 105° C. with stirring to dissolve 9,10-phenanthrenequinone. To the resultant, the crystals of 3,5-dichloro-2-hydrazinopyridine (4.6 g) was added in 30 minutes. After stirring at 105 to 110° C. for one hour, the reaction mixture was filtrated. The filtrated crystals were washed with methanol, and then dried to give intended crystals (5.1 g).

Aufarbeitung

  1. stirringAfter stirring at 105 to 110° C. for one hour
  2. filtrationthe reaction mixture was filtrated
  3. washThe filtrated crystals were washed with methanol
  4. customdried
  5. customto give

Quellen und Nachweise

ORD-Eintrag
ord-5ffcf76dc5404586bdf823c8317970b4
Quelldatensatz
uspto-grants-2003_04
Patentnummer
US06551682B1

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