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
반응 조건
- 온도
- 125 °C
실험 절차
450 parts of polyphosphoric acid containing 85.0% P2O5 are metered into a stirred vessel Then 127.5 parts of 2,5-dianilinoterephthalic acid and 22.5 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 860.8 parts of 85% strength phosphoric acid at 140° C., during which it is hydrolyzed. During this hydrolysis the temperature rises to 160° C. The phosphoric acid concentration after the hydrolysis is 95%. Then 1105 parts of 40% strength phosphoric acid are added dropwise and the suspension is cooled to 120° C. The phosphoric acid concentration thereafter is 70%. The mixture is stirred at 120° C. for 3 hours. The mixture is then cooled to 110° C. and the mixed crystal pigment is filtered off with suction, washed with 70% strength phosphoric acid until the runoff is colorless, washed to neutrality with water, and dried at 80° C. This gives 131 parts of mixed crystal pigment (Pigment Violet 19, γIV phase). At twice the Bragg angle, 2θ, X-ray spectrum shows three strong lines at 6.4°, 13.5° and 26.4°, five moderate lines at 13.3°, 16.9°, 20.5°, 24.0° and 28.3°, and one weak line at 30.1°.
출처 및 근거
- ORD 기록
- ord-7c1a7a3414a9433eb400d6d558d03289
- 출처 데이터셋
- uspto-grants-2001_11
- 특허 번호
- US06312512B1
연결된 노트
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