反应详情

Ethenylidenebisphosphonic acid tetraethyl ester (I, 3.00 g), ethyl acetoacetate (II, 1.4 ml), and DBU (0.25 ml) are heated to 500 in THF (20 ml) for 1.5 hours. The reaction is cooled, diluted with ethyl acetate, filtered through magnesium sulfate and concentrated under reduced pressure. The concentrate is chromatographed eluting with ethyl acetate, ethyl acetate/acetone (1/1). The appropriate fractions are pooled and concentrated to give the title compound, MS (m/e) 430 (M+), 388, 339, 301 and 288; IR (neat) 2984, 1740, 1716, 1478, 1444, 1392, 1368 and 1250 cm- ; NMR (CDCl3) 4.20, 2.43, 2.29, 1.35 and 1.28 δ.

1. temperatureThe reaction is cooled
2. filtrationfiltered through magnesium sulfate
3. concentrationconcentrated under reduced pressure
4. customThe concentrate is chromatographed
5. washeluting with ethyl acetate, ethyl acetate/acetone (1/1)
6. concentrationconcentrated