反应详情

A solution of NaNO2 (0.16 g) in water (2 mL) was added dropwise to an ice-cold solution of 3-[(S)-1-(3′,4′-diamino-biphenyl-4-yl)-ethyl]-(S)-6-(2-hydroxy-2-methyl-propyl)-6-phenyl-[1,3]oxazinan-2-one (0.43 g) in acetic acid (10 mL). The resulting mixture was stirred with cooling for 2 h and at room temperature for another 1 h. Then, water (100 mL) was added and the resulting mixture was extracted with ethyl acetate. The combined organic extracts were washed with saturated aqueous NaHCO3 solution, water, and brine and dried (Na2SO4). The solvent was removed and the residue was purified by chromatography on silica gel (ethyl acetate/MeOH 98:2→80:20) to afford the title compound as a foam-like solid.

1. extractionthe resulting mixture was extracted with ethyl acetate
2. washThe combined organic extracts were washed with saturated aqueous NaHCO3 solution, water, and brine
3. dry with materialdried (Na2SO4)
4. customThe solvent was removed
5. customthe residue was purified by chromatography on silica gel (ethyl acetate/MeOH 98:2→80:20)