9,10-Phenanthrenedione → 10-[6-(2,2,3,3,4,4,5,5-Octafluoropentyloxy)-2-pyridylazo]-9-phenanthrol

HRID 1266926

Reaktionsgleichung

Reaktionsgleichung von HRID 1266926
[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.[NH:17]([C:19]1[CH:24]=[CH:23][CH:22]=[C:21]([O:25][CH2:26][C:27]([F:38])([F:37])[C:28]([F:36])([F:35])[C:29]([F:34])([F:33])[CH:30]([F:32])[F:31])[N:20]=1)[NH2:18]>C(O)(=O)C>[F:38][C:27]([F:37])([C:28]([F:35])([F:36])[C:29]([F:33])([F:34])[CH:30]([F:32])[F:31])[CH2:26][O:25][C:21]1[N:20]=[C:19]([N:17]=[N:18][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])[CH:24]=[CH:23][CH:22]=1

Komponenten

4

Edukt 2

HCID 67639,10-Phenanthrenedione2×HCID 185447822-Hydrazino-6-(2,2,3,3,4,4,5,5-octafluoropentyloxy)pyridine

Produkt 1

HCID 13638834310-[6-(2,2,3,3,4,4,5,5-Octafluoropentyloxy)-2-pyridylazo]-9-phenanthrol

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
110 °C

Versuchsvorschrift

Next, a reaction flask was loaded with acetic acid (54 ml) and 9,10-phenanthrenequinone (3.8 g), and the temperature was raised to 110° C. with stirring to dissolve 9,10-phenanthrenequinone. To this mixture, 2-hydrazino-6-(2,2,3,3,4,4,5,5-octafluoropentyloxy)pyridine (10 g) was added in 30 minutes. After stirring at 110° C. for one hour, the reaction mixture was filtrated. Crystals were stirred in methanol (100 ml) for 30 minutes, filtrated and dried to give intended crystals (5.2 g).

Aufarbeitung

  1. stirringAfter stirring at 110° C. for one hour
  2. filtrationthe reaction mixture was filtrated
  3. stirringCrystals were stirred in methanol (100 ml) for 30 minutes
  4. filtrationfiltrated
  5. customdried
  6. customto give

Quellen und Nachweise

ORD-Eintrag
ord-65e0b6deb2c2449c93641d4701329184
Quelldatensatz
uspto-grants-2003_04
Patentnummer
US06551682B1

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