反应详情

The ketone (II, 4.27 g), ethenylidenebisphosphonic acid tetraethyl ester (I, 3.60 g) and DBU (2 ml) are stirred in THF (30 ml) for 1 hour. The reaction is diluted with ethyl acetate, washed with hydrochloric acid (IN), saturated sodium bicarbonate, and saline, dried with magnesium sulfate, and concentrated under reduced pressure. The product is chromatographed eluting with ethyl acetate/ethyl acetate-acetone 1/1) to give the title compound, MS (m/e) 601, 446, 400, 372 and 155; IR (neat) 2983, 1689, 1599, 1574, 1494, 1477, 1392 and 1254 cm-1 ; NMR (CDCl3) 7.95, 7.8, 7.7, 7.49, 7.28, 7.14, 4.47, 4.20, 3.79, 3.14, 2.83, 2.4, 1.93 and 1.32 δ.

1. washwashed with hydrochloric acid (IN), saturated sodium bicarbonate, and saline
2. dry with materialdried with magnesium sulfate
3. concentrationconcentrated under reduced pressure
4. customThe product is chromatographed
5. washeluting with ethyl acetate/ethyl acetate-acetone 1/1)