反应详情

温度

0 °C

To a solution of (7-hydroxy-2-benzofuranyl)(5-methyl-3-phenyl-4-isoxazolyl)methanone (example 4) (100 mg, 0.31 mmol) in THF (3.1 mL) was added ethanol (19 mg, 24 μL, 0.42 mmol) and triphenylphosphine (109 mg, 0.42 mmoL) at room temperature. The resulting mixture was then cooled to 0° C. and diethyl azodicarboxylate (73 mg, 65 μL, 0.42 mmol) added. The resulting mixture was maintained at 0° C. for 30 min and then allowed to warm up to room temperature overnight. The mixture was then adsorbed onto SiO2 and purification by chromatography (SiO2, heptane:ethyl acetate:=100:0 to 75:25) afforded the title compound (90 mg, 83%) as a white solid. MS m/e: 348.4 [M+H]+.

1. temperatureThe resulting mixture was maintained at 0° C. for 30 min
2. temperatureto warm up to room temperature overnight
3. customThe mixture was then adsorbed onto SiO2 and purification by chromatography (SiO2, heptane:ethyl acetate:=100:0 to 75:25)