反应详情

温度

100 °C

A stirred mixture of 70.8 g (0.15 mol) of 2,4,6-triiodophenol, 39.0 g (0.15 mol) of diethyl bromomalonate and 20.7 g (0.15 mol) of milled anhydrous potassium carbonate in 200 ml of dry dimethylformamide was heated at 100° C. under argon for 5 hours. The mixture was cooled and concentrated in vacuo. The resulting residue was combined with 300 ml of ice-cold water and the oily product was extracted with ethyl acetate (1×300 ml), 3×100 ml). The combined ethyl acetate extracts were dried (MgSO4) and concentrated in vacuo to a dark oil. The oil was purified by chromatography (eluted by hexanes to 20% diethyl ether in hexanes) to yield 60.2 g (64%) of product as a light cream-colored solid.

1. temperatureThe mixture was cooled
2. concentrationconcentrated in vacuo
3. extractionthe oily product was extracted with ethyl acetate (1×300 ml), 3×100 ml)
4. dry with materialThe combined ethyl acetate extracts were dried (MgSO4)
5. concentrationconcentrated in vacuo to a dark oil
6. customThe oil was purified by chromatography (eluted by hexanes to 20% diethyl ether in hexanes)