反应 #55293

ord-ab48e2fc323544fd9da70d48d08406f8

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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.).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04220357uspto-grants-1980_09