2,5-Dianilinoterephthalic acid → Quinacridone

HRID 427191

반응식

HRID 427191 반응식
[NH:1]([C:8]1[CH:16]=[C:15]([C:17](O)=[O:18])[C:14]([NH:20][C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)=[CH:13][C:9]=1[C:10](O)=[O:11])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.ClC1C=C(C=CC=1)NC1C=C(C(O)=O)C(NC2C=CC=C(Cl)C=2)=CC=1C(O)=O>>[CH:24]1[CH:25]=[C:26]2[C:17]([C:15]3[C:14]([NH:20][C:21]2=[CH:22][CH:23]=1)=[CH:13][C:9]1[C:10]([C:7]2[C:2]([NH:1][C:8]=1[CH:16]=3)=[CH:3][CH:4]=[CH:5][CH:6]=2)=[O:11])=[O:18]

참가 물질

3

반응 조건

온도
125 °C

실험 절차

450 parts of polyphosphoric acid containing 85.0% P2O5 are metered into a stirred vessel. Then 135 parts of 2,5-dianilinoterephthalic acid and 15 parts of 2,5-di(3-chloroanilino) terephthalic acid are introduced at 125° C. with stirring and the mixture is heated at 125° C. for 1 hour during which ring closure takes place to form the quinacridone. The reaction mixture is subsequently metered with stirring over 2 minutes (CG: 50%/min) into a mixture of 1607.5 parts of 80% strength phosphoric acid and 50 g of cumene at 115° C., during which it is hydrolyzed. During this hydrolysis the temperature rises to 135° C. The phosphoric acid concentration after the hydrolysis is 87.5%. Then 1209.2 parts of 40% strength phosphoric acid are added dropwise and the suspension is cooled to 110° C. The phosphoric acid concentration thereafter is 70%. Then the cumene is removed by distillation. At 100° C. the mixed crystal pigment is filtered off with suction, washed with 70% strength phosphoric acid until the runoff is coloress, washed to neutrality with water, and dried at 80° C. This gives 125.1 parts of mixed crystal pigment (Pigment Violet 19, γII phase).

출처 및 근거

ORD 기록
ord-4b8a1061047444cf90fe27c381d3eb5f
출처 데이터셋
uspto-grants-2001_11
특허 번호
US06312512B1

연결된 노트

불러오는 중…