Phthalonitrile → Dichlorotitanium phthalocyanine

HRID 321905

反応式

HRID 321905 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.[Ti:11](Cl)(Cl)([Cl:13])[Cl:12]>ClC1C2C(=CC=CC=2)C=CC=1>[Cl:12][Ti:11][Cl:13].[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 2

HCID 7042PhthalonitrileHCID 24193Titanium Tetrachloride

生成物 1

HCID 136368297Dichlorotitanium phthalocyanine

試薬・触媒・溶媒 1

HCID 70031-Chloronaphthalene溶媒

反応条件

温度
225 °C

実験手順

40 g of o-phthalodinitrile, 18 g of titanium tetrachloride and 500 ml of α-chloronaphthalene were heated and stirred under a nitrogen atmosphere at 200 to 250° C. for 3 hours to react them, and after allowed to be cooled to 100 to 130° C., the reaction product was filtrated while hot and washed with 200 ml of α-chloronaphthalene heated to 100° C., so as to obtain a crude product of dichlorotitanium phthalocyanine. The crude product was washed successively with 200 ml of α-chloronaphthalene and 200 ml of methanol at room temperature, and was washed by dispersing in 500 ml of hot methanol for 1 hour. A crude product obtained by filtration was repeatedly washed by dispersing in 500 ml of hot water until the pH becomes 6 to 7, and oxotitanylphthalocyanine crystal was obtained by drying.

後処理

  1. customto react them
  2. temperatureto be cooled to 100 to 130° C.
  3. filtrationthe reaction product was filtrated while hot and
  4. washwashed with 200 ml of α-chloronaphthalene
  5. temperatureheated to 100° C.

出典と根拠

ORDレコード
ord-0523320cd88c4a8ea5da3d383c2c0a8f
出典データセット
uspto-grants-2001_04
特許番号
US06210847B1

関連ノート

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