反应详情

To a solution of 3,5-diiodobenzoic acid (6.8 g, 18.18 mmol) in methanol (200.0 ml) was added CH3SO3H (0.5 ml). The reaction mixture was heated to reflux. After refluxing for 7.5 hours, most of the methanol was removed. Then, water (200.0 ml) was added and a dark-brown solid was collected by filtration. The product was purified by silica gel column chromatography using hexanes/ethyl acetate (8:2) as eluent. The final pure white product was obtained in the amount of 4.2 g (59.2%) by recrystallization from methanol/water:

1. temperatureThe reaction mixture was heated to reflux
2. customwas removed
3. additionThen, water (200.0 ml) was added
4. filtrationa dark-brown solid was collected by filtration
5. customThe product was purified by silica gel column chromatography
6. customThe final pure white product was obtained in the amount of 4.2 g (59.2%) by recrystallization from methanol/water