تفاعل #514373

ord-4b8a1061047444cf90fe27c381d3eb5f

معادلة التفاعل

O=C(O)c1cc(Nc2ccccc2)c(C(=O)O)cc1Nc1ccccc1
2,5-dianilinoterephthalic acid
O=C(O)c1cc(Nc2cccc(Cl)c2)c(C(=O)O)cc1Nc1cccc(Cl)c1
2,5-di(3-chloroanilino) terephthalic acid
O=c1c2ccccc2[nH]c2cc3c(=O)c4ccccc4[nH]c3cc12
quinacridone

ظروف التفاعل

درجة الحرارة
125°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

الإجراء التجريبي

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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06312512B1uspto-grants-2001_11