反应详情

To a stirred solution of 2-(5-chloro-1-benzofuran-3-yl)ethanol (980 mg, 5 mmol) in anhydrous THF (50 ml), triphenylphosphine (1.572 g, 6 mmol), iodine (1.518 g, 6 mmol) and imidazole (408 mg, 6 mmol) were added at room temperature. The reaction mixture was stirred at room temperature for 4 hrs and quenched with water. It was then extracted with chloroform, washed well with 5% Na2S2O3 and the organic layer dried over anhydrous MgSO4. It was filtered and concentrated. The residue was purified by silica-gel column chromatography by eluting it with 30% ethyl acetate:hexane. The product, 2-(5-chloro-1-benzofuran-3-yl)ethyl iodide, was obtained as brown liquid; Yield: 1.2 g (80%); (M+H): 306.

1. customquenched with water
2. extractionIt was then extracted with chloroform
3. washwashed well with 5% Na2S2O3
4. dry with materialthe organic layer dried over anhydrous MgSO4
5. filtrationIt was filtered
6. concentrationconcentrated
7. customThe residue was purified by silica-gel column chromatography
8. washby eluting it with 30% ethyl acetate