反応 #473563

ord-bd1102cf020049879ce49d89a44449ac

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他was evacuated
  2. 2
    workup.ADDITIONfilled with nitrogen twice
  3. 3
    workup.WAITat 120° C. for 2 days
  4. 4
    温度The reaction mixture was then cooled to room temperature
  5. 5
    workup.ADDITIONdiluted with ethyl acetate
  6. 6
    ろ過filtered through silica gel
  7. 7
    濃縮concentrated

実験手順

A mixture of 1H-pyrazole (300 mg, 4.4 mmol), iodonaphthalene (1.1 g, 4.4 mmol), copper (I) iodide (126 mg, 0.66 mmol), Cs2CO3 (2.15 g, 6.6 mmol) in DMF (5 mL) was evacuated and filled with nitrogen twice. The reaction was then stirred at room temperature for 30 minutes and then at 120° C. for 2 days. The reaction mixture was then cooled to room temperature, diluted with ethyl acetate, filtered through silica gel and concentrated to give 1-(naphthalen-1-yl)-1H-pyrazole as pure solid. (800 mg, 93%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08372807B2uspto-grants-2013_02