反应详情

温度

0 °C

Lithium tetrahydroaluminate (20.4 mg, 0.537 mmol) was added to a solution of ethyl (1R,3S)-3-[(6-nitrothieno[3,2-b]pyridin-7-yl)amino]cyclopentanecarboxylate (0.15 g, 0.45 mmol) in tetrahydrofuran (4.0 mL) with stirring at about 0° C. The resulting mixture was kept cold and stirred for 40 min. Fieser workup was performed followed by filtration through Celite and concentrated. The crude was purified using silica gel, eluted with 40-100% EtOAc in hexanes to give 70 mg (50%) of the desired product. LCMS calculated for C13H16N3O3S (M+H)+: m/z=294.1. Found: 294.0.

1. stirringstirred for 40 min
2. filtrationFieser workup was performed followed by filtration through Celite
3. concentrationconcentrated
4. customThe crude was purified
5. washeluted with 40-100% EtOAc in hexanes