反应详情

温度

0 °C

To a solution of trifluoro-methanesulfonic acid 5-hydroxy-5,6,7,8-tetrahydro-naphthalen-2-yl ester (Step B, 11.2 g, 37.9 mmol, 1.0 eq) in THF (150 mL) at RT was added DPPA (Aldrich, 11.1 mL, 51.6 mmol, 1.36 eq). The resulting mixture was cooled to 0° C. and then DBU (Aldrich, 7.7 mL, 51.6 mmol, 1.36 eq) was added slowly through a syringe. The reaction was warmed to RT and stirred over the weekend. The mixture was concentrated in vacuo. The residue was dissolved in EtOAc (400 mL), washed with saturated NH4Cl (twice), H2O, and brine, dried over Na2SO4 and concentrated in vacuo. The crude was purified by flash chromatography (5% EtOAc-hexane) to provide the title compound.

1. temperatureThe reaction was warmed to RT
2. concentrationThe mixture was concentrated in vacuo
3. dissolutionThe residue was dissolved in EtOAc (400 mL)
4. washwashed with saturated NH4Cl (twice), H2O, and brine
5. dry with materialdried over Na2SO4
6. concentrationconcentrated in vacuo
7. customThe crude was purified by flash chromatography (5% EtOAc-hexane)