反応 #999335

ord-8036c311c9f7474e8a9ec5c3ab79236f

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    洗浄The reaction mixture was washed with aqueous ammonium chloride solution
  2. 2
    乾燥subsequently dried over sodium sulfate
  3. 3
    ろ過After filtering sodium sulfate
  4. 4
    濃縮the filtrate was concentrated under reduced pressure

実験手順

To 4-methyl-3-nitro-benzoic acid (730 mg, 4.03 mmol), WSCI (930 mg, 4.85 mmol), HOBt (110 mg, 0.674 mmol) and N-ethylpiperazine (608 μl, 4.79 mmol), dichloromethane (8 ml) was added, followed by stirring for 13 hours. The reaction mixture was washed with aqueous ammonium chloride solution, and subsequently dried over sodium sulfate. After filtering sodium sulfate, the filtrate was concentrated under reduced pressure, to obtain (4-ethyl-piperazin-1-yl)-(4-methyl-3-nitro-phenyl)-methanone (1.06 g, 95%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08022205B2uspto-grants-2011_09