反応 #2126615

ord-f58db48252e74fc08dea53e5262ebfce

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度with reflux under a nitrogen atmosphere for 24 hours
  2. 2
    workup.ADDITIONwas added
  3. 3
    その他The crude product was purified by column chromatography

実験手順

In a 250 ml two-neck flask, 80 ml of N,N-dimethyl formamide (DMF), 2.92 g (6.85 mmol) of 3-(3,6-dibromo-9H-carbazol-9-yl) benzonitrile, 0.98 g (15.08 mmol) of sodium azide (NaN3), 0.81 g (15.08 mmol) of ammonium chloride (NH4Cl), and a stir bar were added. The reaction was carried out with reflux under a nitrogen atmosphere for 24 hours. After the completion of reaction, 20 ml of 10% hydrochloric acid (HCl) was added and a filtering was conducted. The crude product was purified by column chromatography to obtain 3.21 g of a white solid product of 3,6-dibromo-9-(3-2H-tetraazol-5-yl-phenyl)-9H-carbazole (yield: 82.9%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08580396B2uspto-grants-2013_11