反应详情

温度

100 °C

To a stirred solution of 5-[2,4-bis(benzyloxy)-6-(4-nitrophenoxy)phenyl]-N-ethylisoxazole-3-carboxamide (1.45 g, 2.6 mmol) and ammonium chloride (1.4 g, 6.4 mmol, 10 eq.) in dioxane (18 mL) and water (3 mL) was added powered Zn (0.7 g, 10 mmol, 4 eq.). After heating at 100° C. for 2 hours, the solution was filtered and the filtrate was diluted with ethyl acetate and washed with 1 M NaHCO3 solution. After drying, the solvent was removed and the residue was chromatographed on silica gel eluting with hexane/ethyl acetate 3/1, to provide the title compound (0.69 g, 49% yield).

1. filtrationthe solution was filtered
2. additionthe filtrate was diluted with ethyl acetate
3. washwashed with 1 M NaHCO3 solution
4. customAfter drying
5. customthe solvent was removed
6. customthe residue was chromatographed on silica gel eluting with hexane/ethyl acetate 3/1