反应详情

温度

76 °C

Compound 122 (119 mg, 0.39 mmol) was stirred in HOAc (3 mL) with H2O (0.5 mL) and stirred at 76° C. Iron powder (˜325 mesh, 88 mg, 1.56 mmol) was added, and the reaction stirred for 4 h. The solution was concentrated in vacuo, diluted with EtOAc (30 mL), and made basic with sat. NaHCO3. The material was then filtered through Celite, and the organics were separated, dried (MgSO4), and concentrated in vacuo to give 148 mg (66%) of the title compound as a brown oil. MS (ES) [m+H] calc'd for C13H11FN4, 243; found 243.

1. stirringthe reaction stirred for 4 h
2. concentrationThe solution was concentrated in vacuo
3. additiondiluted with EtOAc (30 mL)
4. filtrationThe material was then filtered through Celite
5. customthe organics were separated
6. dry with materialdried (MgSO4)
7. concentrationconcentrated in vacuo