Phthalonitrile → Phthalocyanine

HRID 376813

반응식

HRID 376813 반응식
[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

참가 물질

4

반응물 1

HCID 7042Phthalonitrile

생성물 1

HCID 86280045Phthalocyanine

시약·촉매·용매 2

HCID 24193Titanium Tetrachloride촉매HCID 70031-Chloronaphthalene용매

반응 조건

온도
217.5 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-5b3f35573b28427b807879c342f432f3
출처 데이터셋
uspto-grants-2000_02
특허 번호
US06022656

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