反応 #2168113

ord-01edc6b164a34a429e527641be090554

反応条件

温度
0°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.WAITAfterward, the mixture was left
  2. 2
    workup.WAITto stand at room temperature overnight
  3. 3
    workup.STIRRINGthe mixture was stirred for 1 h
  4. 4
    ろ過then the precipitate was filtered off with suction
  5. 5
    洗浄washed with water
  6. 6
    その他dried
  7. 7
    その他purified chromatographically on silica gel

実験手順

1 g (2.863 mmol) of 2-(3-pentafluorosulfanylphenyl)isoindole-1,3-dione was dissolved at 0° C. in 3.29 ml of concentrated nitric acid, and the mixture was stirred at 0° C. for 2 h. Afterward, the mixture was left to stand at room temperature overnight. The reaction solution was added to 50 g of ice-water and the mixture was stirred for 1 h; then the precipitate was filtered off with suction, washed with water, dried and purified chromatographically on silica gel using toluene as the eluent. 2-(4-Nitro-3-pentafluorosulfanylphenyl)isoindole-1,3-dione having a melting point of 200-203° C. and 2-(2-nitro-5-pentafluorosulfanylphenyl)isoindole-1,3-dione having a melting point of 175-177° C. were obtained in a ratio of 1:2.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07932416B2uspto-grants-2011_04