反应详情

p-Iodobenzenesulfonyl chloride (593 g, 1.96 mol), prepared as described in Example 1(a) above, is dissolved in 2.5 L of acetone and placed in a 5 L three-neck round-bottom flask fitted with a heating mantle, mechanical stirring and a water-cooled condenser. Potassium fluoride (126 g, 2.17 mol) and about 25 mL of water is added and the reaction is heated at reflux for approximately 5 hours. On cooling, the reaction mass is filtered and the solvent removed to provide a crude solid, which on purification, by distillation under high vacuum, affords p-iodobenzenesulfonyl fluoride as a white solid; yield 504 g (90%).

1. customplaced in a 5 L three-neck round-bottom flask
2. customfitted with a heating mantle
3. temperaturethe reaction is heated
4. temperatureat reflux for approximately 5 hours
5. temperatureOn cooling
6. filtrationthe reaction mass is filtered
7. customthe solvent removed
8. customto provide a crude solid, which
9. customon purification
10. distillationby distillation under high vacuum