反応 #55286

ord-f064d3df4da644fe9118044c211883d6

反応条件

温度
95°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度cooled
  2. 2
    その他Recrystallization of the resulting solid
  3. 3
    workup.ADDITIONfrom a mixture of toluene and hexane

実験手順

A mixture of 2-(4-(dimethylamino)benzoyl)benzoic acid (26.8 g.), N,N,N',N'-tetramethyl-m-phenylenediamine (16.4 g.) and acetic anhydride (80 g.) was heated (to 95° C.) during one hour, cooled and poured into dilute hydrochloric acid. The resulting mixture was basified. Recrystallization of the resulting solid from a mixture of toluene and hexane afforded 3-(2,4-bis(dimethylamino)phenyl)-3-(4-(dimethylamino)phenyl)phthalide (I: X=Y4 =(CH3)2N, Y2 =Z4 =Z5 =Z6 =Z7 =H) (m.p. 190°-194° C.).

出典

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