反応 #622412

ord-d34492f763de4fd481d6e7a644e9a208

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONwas added
  2. 2
    抽出Then an extraction
  3. 3
    その他dried

実験手順

In a 250 ml two-neck flask, 60 ml of N,N-dimethyl formamide, 450 mg (1.07 mmol) of 3-(3,6-diphenyl-9H-carbazol-9-yl) benzonitrile, 208.71 mg (3.21 mmol) of sodium azide, 171.73 mg (3.21 mmol) of ammonium chloride, and a stir bar were added. The reaction was carried out at a constant temperature of 100° C. under a nitrogen atmosphere for 38 hours. After the completion of reaction, 10 ml of 10% HCl was added and a filtering was conducted. Then an extraction was conducted with ethyl acetate and water. The organic layer was drawn out and dried to obtain a light orange solid product of 3,6-diphenyl-9-(3-2H-tetraazol-5-yl-phenyl)-9H-carbazole (yield: 85%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08859113B2uspto-grants-2014_10