反应详情

To a solution of benzyl 2-fluoro-3-(1-(6-(2-methoxyethoxy)-1H-indol-3-yl)-2-nitroethyl)phenylcarbamate (3.75 g, 7.39 mmol) and ammonium chloride (5.93 g, 111 mmol) in methanol (148 mL) and tetrahydrofuran (148 mL) under nitrogen was added zinc (7.25 g, 111 mmol). After 3 hr, the reaction was filtered through a pad of CELITE®, rinsed with EtOAc and MeOH. The filtrate was concentrated in vacuo. Water (40 mL) was added followed by saturated aq. NaHCO3 (to pH ˜11 by litmus paper) and extracted with EtOAc (4×50 mL). The organic layers were combined, washed with brine (40 mL), dried over MgSO4, and concentrated in vacuo to give the desired product (3.523 g, 6.35 mmol, 86% yield) as a light tan solid.

1. filtrationthe reaction was filtered through a pad of CELITE®
2. washrinsed with EtOAc and MeOH
3. concentrationThe filtrate was concentrated in vacuo
4. additionWater (40 mL) was added
5. extractionextracted with EtOAc (4×50 mL)
6. washwashed with brine (40 mL)
7. dry with materialdried over MgSO4
8. concentrationconcentrated in vacuo