反应详情

温度

85 °C

3-Phenyl-thiophene-2-carboxylic acid (200 mg, 979 μmol), NEt3 (99.1 mg, 136 μL, 979 μmol) and diphenylphosphoryl azide (275 mg, 215 μL, 999 μmol) were dissolved in tert-BuOH. The solution was stirred at 85° C. for 5 h followed by RT overnight. The formed suspension was filtered and the filter cake was washed with a small amount of tert-BuOH. The filtrate was diluted with EtOAc, washed with H2O and brine. The organic layers were dried over Na2SO4 and concentrated in vacuo. The crude material was purified by flash chromatography (0% to 18% EtOAc in n-heptane) to give the title compound as a yellow solid (0.122 g, 45%). MS (ESI): m/z=276.2 [M+H]+.

1. waitfollowed by RT overnight
2. filtrationThe formed suspension was filtered
3. washthe filter cake was washed with a small amount of tert-BuOH
4. additionThe filtrate was diluted with EtOAc
5. washwashed with H2O and brine
6. dry with materialThe organic layers were dried over Na2SO4
7. concentrationconcentrated in vacuo
8. customThe crude material was purified by flash chromatography (0% to 18% EtOAc in n-heptane)