تفاعل #55299

معادلة التفاعل

2-(2,4-bis(dimethylamino)benzoyl)-4-(dimethylamino)benzoic acid

N,N,N',N'-tetramethyl-m-phenylenediamine

acetic anhydride

→

3,3-bis(2,4-bis(dimethylamino)phenyl)-5-(dimethylamino)phthalide

المذيبات

hydrochloric acid

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwarming
2. 2
   ترشيحfiltered
3. 3
   أخرىCrystallization of the product from toluene

الإجراء التجريبي

A mixture of 2-(2,4-bis(dimethylamino)benzoyl)-4-(dimethylamino)benzoic acid or the 5-(dimethylamino) isomer thereof (10 g.), N,N,N'-tetramethyl-m-phenylenediamine (2.30 g.) and acetic anhydride (50 ml.) was warmed (at 30°-35° C.) during one hour. More N,N,N',N'-tetramethyl-m-phenylenediamine (1.15 g.) was added and warming was continued. The mixture was diluted with dilute hydrochloric acid (10%) and ice and filtered. The filtrate was made alkaline. Crystallization of the product from toluene afforded 3,3-bis(2,4-bis(dimethylamino)phenyl)-5-(dimethylamino)phthalide (I: X=Y2 =Y4 =Z5 =(CH3)2N, Z4 =Z6 =Z7 =H) (m.p. 188°-192° C.) or the 6-(dimethylamino) isomer thereof.

المصدر