反应详情

To a mixture of 4-azido-5-bromo-2-(2,4-dichlorophenylamino)-3-fluorobenzoic acid methyl ester (2.05 g, 4.72 mmol) in AcOH-CH2Cl2 (10-30 mL) was added Zn dust (1.59 g, 24.3 mmol) at 0° C. The reaction mixture was warmed to room temperature. The resulting mixture was stirred for 1 hour. The reaction mixture was diluted with CH2Cl2, and washed with water, saturated aqueous NaHCO3 (2×), water, and brine. The organic layer was dried over MgSO4, filtered, and concentrated in vacuo to give the crude material which was purified by silica gel flash column chromatography(3 to 5% EtOAc in hexanes) to afford the desired product (1.24 g, 64%).

1. washwashed with water, saturated aqueous NaHCO3 (2×), water, and brine
2. dry with materialThe organic layer was dried over MgSO4
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customto give the crude material which
6. customwas purified by silica gel flash column chromatography(3 to 5% EtOAc in hexanes)