反应详情

A heterogeneous solution of benzyl 2-methyl-3-(1-(6-morpholino-1H-indol-3-yl)-2-nitroethyl)phenylcarbamate (1.8743 g, 3.64 mmol), ammonium chloride (2.92 g, 54.6 mmol) and zinc (3.57 g, 54.6 mmol) in THF (Ratio: 1.000, Volume: 79 ml) and methanol (Ratio: 1.000, Volume: 79 ml) was stirred under nitrogen for 2.5 hr. EtOAc (60 mL) was added, and the solution was filtered through a pad of CELITE®. The filtrate was concentrated in vacuo; the residue was dissolved in water (50 mL) and EtOAc (75 mL). After separation of the layers, the aqueous layer was extracted with EtOAc (2×75 mL). The organic layers were combined, dried over MgSO4, and concentrated in vacuo to give the desired product (1.4934 g, 3.08 mmol, 85% yield) as a tan solid.

1. filtrationthe solution was filtered through a pad of CELITE®
2. concentrationThe filtrate was concentrated in vacuo
3. dissolutionthe residue was dissolved in water (50 mL)
4. customAfter separation of the layers
5. extractionthe aqueous layer was extracted with EtOAc (2×75 mL)
6. dry with materialdried over MgSO4
7. concentrationconcentrated in vacuo