反应详情

温度

120 °C

A 10 mL microwave vessel equipt with a stirbar was charged with N′-acetyl-3-morpholino-5-nitrobenzohydrazide (0.250 g, 0.811 mmol), Burgess reagent (0.97 g, 4.05 mmol), and dichloroethane (4 mL). The red solution was heated in a microwave at 120° C. for 20 minutes, then concd. The resulting residue was partitioned between EtOAc and water, and the organic layer washed with 1 N HCl, 1 N sodium hydroxide, and brine, then dried over magnesium sulfate and concd. This afforded a crude material that was purified by column chromatography (silica; 0-75% EtOAc in hexanes), providing 4-(3-(5-methyl-1,3,4-oxadiazol-2-yl)-5-nitrophenyl)morpholine as a yellow amorphous solid. Mass Spectrum (ESI) m/e=291.1 (M+1).

1. customThe resulting residue was partitioned between EtOAc and water
2. washthe organic layer washed with 1 N HCl, 1 N sodium hydroxide, and brine
3. dry with materialdried over magnesium sulfate and concd
4. customThis afforded a crude material that
5. customwas purified by column chromatography (silica; 0-75% EtOAc in hexanes)