9,10-Phenanthrenedione → 10-[3-Chloro-5-(trifluoro-methyl)-2-pyridylazo]-9-phenanthrol

HRID 1266918

Reaktionsgleichung

Reaktionsgleichung von HRID 1266918
[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:28][NH2:29])=[N:20][CH:21]=[C:22]([C:24]([F:27])([F:26])[F:25])[CH:23]=1>C(O)(=O)C>[Cl:17][C:18]1[C:19]([N:28]=[N:29][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]([C:24]([F:27])([F:25])[F:26])[CH:23]=1

Komponenten

4

Edukt 2

HCID 67639,10-Phenanthrenedione2×HCID 12726913-Chloro-2-hydrazinyl-5-(trifluoromethyl)pyridine

Produkt 1

HCID 13571851310-[3-Chloro-5-(trifluoro-methyl)-2-pyridylazo]-9-phenanthrol

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
100 °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 100° C. with stirring to dissolve 9,10-phenanthrenequinone. To the resultant, the crystals of 3-chloro-2-hydrazino-5-(trifluoromethyl)-pyridine (5.0 g) was added in 30 minutes. After stirring at 100 to 105° C. for one hour, the reaction mixture was filtrated. After being washed with methanol, the obtained crystals were dried to give intended crystals (5.6 g).

Aufarbeitung

  1. stirringAfter stirring at 100 to 105° C. for one hour
  2. filtrationthe reaction mixture was filtrated
  3. washAfter being washed with methanol
  4. customthe obtained crystals were dried
  5. customto give

Quellen und Nachweise

ORD-Eintrag
ord-d13af6f1ad5747ef991459ec5268d43d
Quelldatensatz
uspto-grants-2003_04
Patentnummer
US06551682B1

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