反応 #55290

反応方程式

hydrochloric acid

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

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

acetic anhydride

→

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

反応条件

後処理

1. 1
   温度was warmed (at 25°-35° C.) during two to three hours
2. 2
   ろ過filtered with a filter aid
3. 3
   抽出The filter cake was extracted with hot toluene
4. 4
   抽出Dilution of the toluene extract with hexane

実験手順

A mixture of crude 2-(2,4-bis(dimethylamino)benzoyl)benzoic acid (7 g.), N,N,N',N'-tetramethyl-m-phenylenediamine (1.64 g.) and acetic anhydride was warmed (at 25°-35° C.) during two to three hours, then poured into dilute hydrochloric acid (10%). The resulting mixture was basified and filtered with a filter aid. The filter cake was extracted with hot toluene. Dilution of the toluene extract with hexane afforded 3,3-bis(2,4-bis(dimethylamino)phenyl)phthalide (I: X=Y2 =Y4 =(CH3)2N, Z4 =Z5 =Z6 =Z7 =H) (m.p. 186°-188° C.).

出典