반응 #473563

ord-bd1102cf020049879ce49d89a44449ac

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타was evacuated
  2. 2
    workup.ADDITIONfilled with nitrogen twice
  3. 3
    workup.WAITat 120° C. for 2 days
  4. 4
    온도The reaction mixture was then cooled to room temperature
  5. 5
    workup.ADDITIONdiluted with ethyl acetate
  6. 6
    여과filtered through silica gel
  7. 7
    농축concentrated

실험 절차

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%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08372807B2uspto-grants-2013_02