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Synthesis of 1: 5 mmol of ferrocene (0.93 g, 5 mmol, previously purified via sublimation, was suspended in 15 mL of dry hexane. A 1.6 M solution of n-BuLi in hexane/cyclohexane (6.5 mL, 10.4 mmol) was added dropwise, followed by addition of tmeda (0.78 mL, 5.2 mmol, The reaction mixture was stirred at room temperature and under nitrogen for 16 h, to give(1,1′-Fc) Li2(tmcda)2/3, which was used without further purification. A solution of Cu5Mes5·C 6H5CH3(1.00 g, 1 mmol, prepared according to literature procedures (Tsuda, T, Yazawa, T, Watanabe, K, Fujii, T, Saegusa, T. J. Org. Chem. 1981, 46, 192-194, in toluene (12 mL) was added to the solution of (1,1′-Fe)Li2 to yield an orange precipitate. The precipitate was dissolved by addition of 5 mL of THF and heating to 60 °C to give a dark brown solution, from which a small quantity of orange-brown
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2 to yield an orange precipitate. The precipitate was dissolved by addition of 5 mL of THF and heating to 60 °C to give a dark brown solution, from which a small quantity of orange-brown crystals of 1 were obtained after 3 days at room temperature. We were unable to obtain 1 in pure form due to contamination from mesityl-containing byproducts (see text for full Discussion).
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20
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0001366924
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(a) Malessa, M.; Heck, J.; Kopf, J.; Garcia, M. H. Eur, J. Inorg. Chetn. 2006, 857-867.
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68949168149
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6dmso): δ -1.04.
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6dmso): δ -1.04.
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26
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34250771010
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(a) Mulvey, R. E.; Mongin, F.; Uchiyama, M.; Kondo, Y. Angew. Chem., Int. Ed. 2007, 46, 3802-3824.
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0034683119
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Boche, G.9
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29
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68949182223
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2 (2.05 mL, 20 mmol) was subsequently added to the dark red mixture at -78 °C, before warming to room temperature and stirring for 12 h. The solid was filtered off, washed with copious amounts of ammonia (6% solution) and distilled water, and dried under vacuum.
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2 (2.05 mL, 20 mmol) was subsequently added to the dark red mixture at -78 °C, before warming to room temperature and stirring for 12 h. The solid was filtered off, washed with copious amounts of ammonia (6% solution) and distilled water, and dried under vacuum.
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