反応 #62616

ord-5f948ac41b9445e7bc809fe917270260

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過The mixture was then filtered under nitrogen
  2. 2
    濃縮concentrated
  3. 3
    その他to remove solvent at 55° C.

実験手順

To the solution of 2-(5-chloro-7-nitroindolin-1-yl)benzamide of Example 1b (10 gm, 26.5 mmoles) in dimethylformamide (DMF) [100 ml] and ethanol (100 ml) was added 1% Pt/carbon (2.0 gm). The mixture was shaken under hydrogen (59 psi) for 41/2 hours. The mixture was then filtered under nitrogen and concentrated to remove solvent at 55° C. and high vacuum to give a solid (9.1 gm). Recrystallization from chloroform twice afforded 2-(5-chloro-7-aminoindolin-1-yl)benzamide, (4.3 gm, 47.3%), m.p. 199°-201° C. dec.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04761412uspto-grants-1988_08