反应 #2605666
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07566786B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Iodine (1 g) was added to a stirred solution of 3-[(dimethylamino)carbonylbenzenesulfonyl chloride (2 g) (Borthwick et al, J. Med. Chem 2002, 45(1), 1-18) and triphenylphosphine (8.4 g) in 1,4-dioxane at 0° C. The mixture was stirred for 0.5 h at ambient temperature. The mixture was poured into a sodium sulphite solution (50 ml), extracted into ethyl acetate (2×30 ml) and washed with 2N sodium hydroxide solution (2×40 ml). The alkaline extracts were acidified and re-extracted into dichloromethane (3×50 ml). The extracts were washed with water (100 ml), dried (Na2SO4) and evaporated to give the title compound as a colourless solid (1.1 g). extracted into ethyl acetate (2×30 ml) washed with 2N sodium hydroxide solution (2×40 ml) re-extracted into dichloromethane (3×50 ml) The extracts were washed with water (100 ml) dried (Na2SO4) evaporated
来源 ID: ord-14e572f5d30844efa61ff553d50f8b4c