反应详情

To a stirred solution of ethyl 6-(bis(tert-butoxycarbonyl)amino)nicotinate 115 (300 g, 819 mmol) in THF (1.2 L) was added LiAlH4 (57.6 g, 1.51 mol) in THF (3 L) over a period of 30 min at 0° C. The reaction mixture was stirred for 6 h, and H2O (30.0 ml) and 10% NaOH solution (60.0 mL) were added. The solids were removed by filtration and the filtrate was dried (Na2SO4) and concentrated. The crude residue was purified by flash chromatography (CH2Cl2; MeOH=40:1) to give 116 (85.0 g, 46% yield).

1. customThe solids were removed by filtration
2. dry with materialthe filtrate was dried (Na2SO4)
3. concentrationconcentrated
4. customThe crude residue was purified by flash chromatography (CH2Cl2; MeOH=40:1)