反応 #9458

ord-ba70021346be4b7b8d28ff373488a299

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONpoured into 250 mL
  2. 2
    その他crushed ice
  3. 3
    ろ過The resulting precipitate was collected by filtration
  4. 4
    洗浄washed with H2O
  5. 5
    その他dried under vacuum for 2 h

実験手順

A solution of phosphorous oxychloride (3.1 g, 20 mmol) in anhydrous N,N-dimethylformamide (DMF, 14 mL) was added to a suspension of 3-nitro-7-phenylquinolin-4-ol (5.0 g, 18.8 mmol) in 80 mL of DMF over 3 min. The reaction was allowed to stir for 1.5 h and then poured into 250 mL crushed ice. The resulting precipitate was collected by filtration, washed with H2O, and dried under vacuum for 2 h. The crude 4-chloro-3-nitro-7-phenylquinoline thus obtained was used without further purification.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07091214B2uspto-grants-2006_08