反应详情

A solution of 2-iodobenzenesulphonyl chloride (obtained as described in J. Org. Chem. 1977, 42, 3265) (8.28 g) and 4-nitrophenol (3.81 g) in pyridine (50 ml) was heated at 100° C. for 3 hours. Volatile material was removed by evaporation and water (200 ml) was added to the residue. The mixture was extracted with ethyl acetate (2×200 ml) and the combined extracts were washed with 1M hydrochloric acid (2×200 ml) and dried (MgSO4). Solvent was removed by evaporation and the residue was recrystallised from a mixture of ethyl acetate and hexane to give 4-nitrophenyl 2-iodobenzenesulphonate (7.83 g), m.p. 131-133° C.; mass spectrum (+ve CI): 405 (M+).

1. customVolatile material was removed by evaporation and water (200 ml)
2. additionwas added to the residue
3. extractionThe mixture was extracted with ethyl acetate (2×200 ml)
4. washthe combined extracts were washed with 1M hydrochloric acid (2×200 ml)
5. dry with materialdried (MgSO4)
6. customSolvent was removed by evaporation
7. customthe residue was recrystallised from a mixture of ethyl acetate and hexane