反応 #4329

ord-dbe92f0c312a4853a6a2bebab89efc08

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他rises to 70° C
  2. 2
    温度The temperature is maintained at 70°-78° C. for 2 hours
  3. 3
    その他the expected product precipitates
  4. 4
    ろ過After filtration
  5. 5
    洗浄washing to neutrality the product
  6. 6
    その他is recrystallized from 450 ml of ethanol

実験手順

15 ml of water are added, with due care, to 115 ml of concentrated sulphuric acid; the temperature rises to 70° C. 0.105 mole (46 g) of 2,5-dibromo-4-nitro-N-benzenesulphonylaniline are then added. The temperature is maintained at 70°-78° C. for 2 hours. The reaction mixture is poured into 1 kg of ice and water; the expected product precipitates. After filtration and washing to neutrality the product is recrystallized from 450 ml of ethanol. It melts at 178° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04725283uspto-grants-1988_02