Phthalonitrile → Phthalocyanine

HRID 568328ノート

反応式

HRID 568328 の反応式
[CH:1]1[CH:6]=[C:5]([C:7]#[N:8])[C:4]([C:9]#[N:10])=[CH:3][CH:2]=1>ClC1C2C(=CC=CC=2)C=CC=1.[Ti](Cl)(Cl)(Cl)Cl>[CH:1]1[CH:2]=[CH:3][C:4]2[C:5](=[C:7]3[N:8]=[C:7]4[N:10]=[C:9]([C:4]5[CH:3]=[CH:2][CH:1]=[CH:6][C:5]=54)[N:10]=[C:9]4[NH:8][C:7]([C:5]5[CH:6]=[CH:1][CH:2]=[CH:3][C:4]=54)=[N:10][C:9]4=[N:8][C:7]([C:5]5[CH:6]=[CH:1][CH:2]=[CH:3][C:4]=54)=[N:10][C:9]=2[NH:8]3)[CH:6]=1

参加物

4

反応物 1

HCID 7042Phthalonitrile

生成物 1

HCID 86280045Phthalocyanine収率 44.8%

試薬・触媒・溶媒 2

HCID 24193Titanium Tetrachloride触媒HCID 70031-Chloronaphthalene溶媒

実験手順

Titanium tetrachloride (18 g) and phthalodinitrile (40 g) were agitated in α-chloronaphthalene (500 ml) at 240°-250° C. under a nitrogen stream. After completion of the reaction, the product dichlorotitanium phthalocyanine was recovered by filtration. The recovered dichlorotitanium phthalocyanine was heated under reflux for 1 hour together with concentrated aqueous ammonia (300 ml) and pyridine (300 ml) so as to obtain the end compound, α-type titanyl phthalocyanine (18 g). This compound was thoroughly washed in a Soxhlet extractor first with N,N-dimethylformamide, then with acetone.

後処理

  1. customAfter completion of the reaction
  2. filtrationthe product dichlorotitanium phthalocyanine was recovered by filtration
  3. temperatureThe recovered dichlorotitanium phthalocyanine was heated
  4. temperatureunder reflux for 1 hour together with concentrated aqueous ammonia (300 ml) and pyridine (300 ml) so as

出典と根拠

ORDレコード
ord-eb3258a64de746ab87fdd996c59208e0
出典データセット
uspto-grants-1988_03
特許番号
US04728592

反応ノート

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