反应详情

A mixture of 2,4,6-triiodophenol (2.0 g, 4.24 mmol), 2-propylvaleroyl chloride (2.5 ml, 12.7 mmol, 3 eq) and 4-dimethylaminopyridine (DMAP; 20 mg) in 20 ml of acetonitrile was refluxed under argon overnite. The reaction mixture was cooled and poured into excess aqueous sodium bicarbonate and then extracted with dichloromethane. The dichloromethane extract was dried over magnesium sulfate, filtered, and evaporated to give the crude product (2.42 mmol, 95%) as a pink solid. Recrystallization from ethyl acetate gave 1.75 g (68%) of pure product, mp 99°-101° C.

1. temperaturewas refluxed under argon overnite
2. temperatureThe reaction mixture was cooled
3. extractionextracted with dichloromethane
4. extractionThe dichloromethane extract
5. dry with materialwas dried over magnesium sulfate
6. filtrationfiltered
7. customevaporated
8. customto give the crude product (2.42 mmol, 95%) as a pink solid
9. customRecrystallization from ethyl acetate