反应详情

A mixture of 1-(4-chlorobenzo[b]thiophen-2-yl]ethan-1-one (1.67 g), phenyltrimethylammonium tribromide (2.98 g) and tetrahydrofuran (40 ml) was stirred under nitrogen at ambient temperature for 22.5 hours then it was filtered and diluted with water (150 ml). The product was extracted into dichloromethane (3×30 ml), the combined extracts were dried (MgSO4) and the solvents were removed in vacuo. The residue was purified by flash chromatography over silica using dichloromethane as eluant. Appropriate fractions were combined and the solvents removed in vacuo to leave 2-bromo-1-(4-chlorobenzo[b]thiophen-2-yl]ethan-1-one (1.65 g) as an off-white solid, m.p. 116-118° C.

1. filtrationit was filtered
2. additiondiluted with water (150 ml)
3. extractionThe product was extracted into dichloromethane (3×30 ml)
4. dry with materialthe combined extracts were dried (MgSO4)
5. customthe solvents were removed in vacuo
6. customThe residue was purified by flash chromatography over silica
7. customthe solvents removed in vacuo