反応 #4328

ord-617bfdd769eb46abb48d202834543d87

溶媒

反応条件

温度
90°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONare added
  2. 2
    温度The reaction mixture, cooled beforehand
  3. 3
    その他the expected product precipitates
  4. 4
    ろ過It is filtered off
  5. 5
    洗浄washed to neutrality
  6. 6
    その他recrystallized from acetic acid

実験手順

To 250 ml of acetic acid, diluted with 130 ml of water, are added: 1.5 g of sodium nitrite, 0.13 mole of 2,5-dibromo-N-benzenesulphonylaniline prepared in the previous stage and 0.78 mole (32.5 ml) of nitric acid (d=1.52). The reaction mixture is heated for 1 hour at 90° C. The reaction mixture, cooled beforehand, is poured onto 1 kg of ice and the expected product precipitates. It is filtered off, washed to neutrality and then recrystallized from acetic acid; it melts at 148° C.

出典

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