反应详情

温度

60 °C

To a solution of 1H-indole-3-carboxylic acid (500 mg) in tetrahydrofuran (10 mL) were added triethylamine (0.519 mL) and diphenylphosphoryl azide (0.802 mL) at ambient temperature. The mixture was stirred at 60° C. for 2 hours. Ethyl acetate (10 mL) was added to the mixture at room temperature, and then the organic layer was washed with saturated sodium bicarbonate aqueous solution×2, water and brine, dried over magnesium sulfate, and concentrated in vacuo. The residual solid was recrystallized from ethyl acetate (2 mL). The crystals were washed with n-hexane/chloroform (3:1, 1 mL). The crystals were recrystallized from ethyl acetate again to afford 1H-indole-3-carbonyl azide (192 mg) as white crystals.

1. washthe organic layer was washed with saturated sodium bicarbonate aqueous solution×2, water and brine
2. dry with materialdried over magnesium sulfate
3. concentrationconcentrated in vacuo
4. customThe residual solid was recrystallized from ethyl acetate (2 mL)
5. washThe crystals were washed with n-hexane/chloroform (3:1, 1 mL)
6. customThe crystals were recrystallized from ethyl acetate again