反应详情

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).

1. extractionextracted into ethyl acetate (2×30 ml)
2. washwashed with 2N sodium hydroxide solution (2×40 ml)
3. extractionre-extracted into dichloromethane (3×50 ml)
4. washThe extracts were washed with water (100 ml)
5. dry with materialdried (Na2SO4)
6. customevaporated