Phthalonitrile → Phthalocyanine

HRID 376813

Reaktionsgleichung

Reaktionsgleichung von HRID 376813
[C:1](#[N:10])[C:2]1[C:3](=[CH:6][CH:7]=[CH:8][CH:9]=1)[C:4]#[N:5]>ClC1C2C(=CC=CC=2)C=CC=1.[Ti](Cl)(Cl)(Cl)Cl>[CH:7]1[CH:8]=[CH:9][C:2]2[C:3](=[C:4]3[N:5]=[C:4]4[N:10]=[C:1]([C:2]5[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=54)[N:10]=[C:1]4[NH:5][C:4]([C:3]5[CH:6]=[CH:7][CH:8]=[CH:9][C:2]=54)=[N:10][C:1]4=[N:5][C:4]([C:3]5[CH:6]=[CH:7][CH:8]=[CH:9][C:2]=54)=[N:10][C:1]=2[NH:5]3)[CH:6]=1

Komponenten

4

Edukt 1

HCID 7042Phthalonitrile

Produkt 1

HCID 86280045Phthalocyanine

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 24193Titanium TetrachlorideKatalysatorHCID 70031-ChloronaphthaleneLösungsmittel

Reaktionsbedingungen

Temperatur
217.5 °C

Versuchsvorschrift

Phthalonitrile (1100 grams) and titanium tetrachloride (813 grams) were suspended in 6800 milliliters (ml) of 1-chloronaphthalene and heated to 215-220° C. and maintained for 2.5 hours at this temperature. The reaction mixture was cooled to 140° C., and the dark solid was collected and washed with acetone and methanol. After drying, the dark blue solid (1090 grams) was slurried twice in refluxing 10 liters of distilled water for two hours, filtered hot each time, and washed with acetone to yield crude phthalocyanine. The X-ray diffraction spectrum exhibits major peaks of the Bragg angle at 7.5, 8.3, 10.5, 12.7, 14.2, 14.6, 18.9, 22.1, 24.3, 26.1, and 29.9 (all +/-0.2 degrees).

Aufarbeitung

  1. temperaturemaintained for 2.5 hours at this temperature
  2. temperatureThe reaction mixture was cooled to 140° C.
  3. customthe dark solid was collected
  4. washwashed with acetone and methanol
  5. customAfter drying
  6. temperaturein refluxing 10 liters of distilled water for two hours
  7. filtrationfiltered hot each time
  8. washwashed with acetone

Quellen und Nachweise

ORD-Eintrag
ord-5b3f35573b28427b807879c342f432f3
Quelldatensatz
uspto-grants-2000_02
Patentnummer
US06022656

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