反応 #1244513

ord-a6e7f7fdd480427a9c040b63899344fd

溶媒

反応条件

温度
110°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過the reaction mixture was filtered through celite
  2. 2
    workup.ADDITIONThe filtrate was diluted with water and product
  3. 3
    抽出was extracted with dichloromethane
  4. 4
    その他The organic layer was evaporated
  5. 5
    その他the crude product was purified by column chromatography

実験手順

1,2,3-Triazole (5 g), 2-bromo pyridine (8.5 ml) and copper iodide (0.68 g) was taken in dry DMF under Nitrogen atmosphere. 1,2-(N,N-dimethyl) cyclohexyl diamine (1.02 g) and potassium phosphate (30.73 g) was added into above mixture. The reaction mixture was reflux at 110° C. for over night. TLC was checked no starting material and the reaction mixture was filtered through celite. The filtrate was diluted with water and product was extracted with dichloromethane. The organic layer was evaporated and the crude product was purified by column chromatography using 60-120 silica gel and pet ether \ ethyl acetate as eluent to give compound 2-(1H-1,2,3-triazol-1-yl)pyridine as white solid.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07807671B2uspto-grants-2010_10