反应详情

温度

10 °C

To an ethylene glycol (5 mL) suspension of (5-[1,3]-dioxolan-2-yl-benzofuran-2-yl)-(4-fluoro-phenyl)-methanone (370 mg, 1.18 mmol) were added hydrazine monohydrate (165 mg, 2.8 mmol) and potassium hydroxide (152 mg, 2.71 mmol). After stirring this suspension for 2 hours at 10° C., this suspension was further stirred for 1 hour at 160° C. After allowing the reaction mixture to cool on standing, sat. NaCl was poured thereinto followed by extraction with ethyl acetate. The organic layer was separated followed by drying over anhydrous magnesium sulfate and concentrating under a reduced pressure. The resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=5:1) to obtain 5-[1,3]-dioxolan-2-yl-2-(4-fluoro-benzyl)-benzofuran (151 mg, 43%).

1. stirringthis suspension was further stirred for 1 hour at 160° C
2. temperatureto cool
3. extractionthereinto followed by extraction with ethyl acetate
4. customThe organic layer was separated
5. dry with materialby drying over anhydrous magnesium sulfate
6. concentrationconcentrating under a reduced pressure
7. customThe resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate=5:1)