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To 1 mmol (0.292 g) of zirconocene dichloride dissolved in 5 mL of dry THF was added 2 mmol (1.25 mL of n-BuLi 1.6 M in hexane) dropwise at -78 °C. The mixture was stirred for 3 h, then 0.9 mmol of 1-alkynylphosphonate was added, and the mixture was slowly warmed to 25 °C and stirred overnight. The mixture was worked up with dilute aqueous HCl, and the vinylphosphonate was extracted in ether and separated on a silica gel column (80% petroleum ether: 20% ethyl acetate).
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