反応 #55293

反応方程式

hydrochloric acid

2-(2-ethoxy-4-(diethylamino)benzoyl)benzoic acid

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

acetic anhydride

→

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

反応条件

後処理

1. 1
   温度was heated (70°-75° C.) during one hour
2. 2
   その他Recrystallization of the resulting red precipitate from hexane

実験手順

A mixture of 2-(2-ethoxy-4-(diethylamino)benzoyl)benzoic acid (6.82 g.), N,N,N',N'-tetramethyl-m-phenylenediamine (2.80 g.) and acetic anhydride (20 g.) was heated (70°-75° C.) during one hour, let stand overnight and poured into dilute hydrochloric acid. The resulting mixture was basified. Recrystallization of the resulting red precipitate from hexane followed by slurrying in alkaline water afforded 3-(2,4-bis(dimethylamino)phenyl)-3-(2-ethoxy-4-(diethylamino)phenyl)phthalide (I: X=(CH3)2N, Y2 =CH3CH2O, Y4 =(CH3CH2)2N, Z4 =Z5 =Z6 =Z7 =H) (m.p. 146°-150° C.).

出典