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note
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2Zr(H)Cl was injected THF (5 ml), followed by the addition of terminal alkynes (1.2 mmol) at room temperature. The mixture was stirred for 20 min to yield a clear solution. Then were added dialkyl chlorophosphates (1.2 mmol) and CuBr (0.15 mmol), and stirred 3 hr. The solvent was removed by rotary evaporator under reduced pressure. The residue was extracted with light petroleum ether (36 ml) and filtered though a short plug of silica gel. After removal of solvent, the residue was purified by preparative TLC on silica gel eluting with light petroleum ether (30-60 °C).
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