2,5-Di-p-toluidinoterephthalic acid → Quinacridone

HRID 1065969

反応式

HRID 1065969 の反応式
[C:1]1(C)[CH:6]=[CH:5][C:4]([NH:7][C:8]2[CH:16]=[C:15](C(O)=O)[C:14](NC3C=CC(C)=CC=3)=[CH:13][C:9]=2[C:10](O)=[O:11])=[CH:3][CH:2]=1.ClC1C=CC([NH:34][C:35]2[CH:43]=[C:42](C(O)=O)[C:41](NC3C=CC(Cl)=CC=3)=[CH:40][C:36]=2[C:37](O)=[O:38])=CC=1>>[CH:1]1[CH:6]=[C:5]2[C:10]([C:9]3[C:8]([NH:7][C:4]2=[CH:3][CH:2]=1)=[CH:16][C:15]1[C:37]([C:36]2[C:35]([NH:34][C:14]=1[CH:13]=3)=[CH:43][CH:42]=[CH:41][CH:40]=2)=[O:38])=[O:11]

参加物

3

反応物 2

HCID 825242,5-Di-p-toluidinoterephthalic acidHCID 1705571,4-Benzenedicarboxylic acid, 2,5-bis[(4-chlorophenyl)amino]-

生成物 1

HCID 13976Quinacridone

反応条件

温度
125 °C

実験手順

A stirred vessel is charged with 1000 parts of polyphosphoric acid containing 85.0% P2O5. Then 75 parts of 2,5-di(4-toluidino)terephthalic acid and 60 parts of 2,5-di(4-chloroanilino)terephthalic acid are introduced at 90° C. with stirring over 25 minutes. During this addition the temperature rises to 120° C. The mixture is heated to 125° C. and stirred at 125° C. for 1 hour, and ring closure takes place to form the quinacridone. The reaction mixture is subsequently metered into a static mixer, model Kenics KMR (length: 10 cm, diameter: 9 mm, 8 elements, supplier: H. Ott, Neckargmünd) with a throughput of 3.3 parts by volume per hour in a volume flow of 27 parts by volume per hour of 70% strength phosphoric acid at 95° C. and is hydrolyzed in 0.9 second (a precipitate is formed). During hydrolysis, the temperature rises to 118° C. Following the hydrolysis the phosphoric acid strength is 77.7%. This gives 4905 parts of crude pigment suspension. After cooling to 60° C., the crude pigment suspension is filtered off with suction, washed to neutrality with water and dried at 80° C.

後処理

  1. additionDuring this addition the temperature
  2. customrises to 120° C
  3. stirringstirred at 125° C. for 1 hour

出典と根拠

ORDレコード
ord-2e527bc5452b459e9b2815316c530f33
出典データセット
uspto-grants-2001_06
特許番号
US06241814B1

関連ノート

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