Реакция #55293

ord-ab48e2fc323544fd9da70d48d08406f8

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураwas heated (70°-75° C.) during one hour
  2. 2
    ДругоеRecrystallization of the resulting red precipitate from hexane

Методика

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.).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04220357uspto-grants-1980_09