反応 #5023

ord-fa8c1a5973204abeab956b536c71aec8

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度to refluxing for 5 hours with vigorous stirring
  2. 2
    ろ過The reaction mixture was filtered by suction while hot
  3. 3
    その他to remove insoluble matter
  4. 4
    濃縮the filtrate thereof was concentrated
  5. 5
    温度cooled

実験手順

To a mixed solution of ethanol (400 ml) and water (100 ml), were added N-acetyl-5-bromo-7-nitroindoline (133.1 g), iron powder (10 mesh; 75 g) and concentrated hydrochloric acid (5 ml), and the mixture was subjected to refluxing for 5 hours with vigorous stirring. The reaction mixture was filtered by suction while hot to remove insoluble matter, and then the filtrate thereof was concentrated and cooled on standing to give the intended compound 38.3 g (32.2%) as a brown needle crystal. M.P.: 154°-155° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05242912uspto-grants-1993_09