Chlorotrimethylsilane → Silane, 2,4-cyclopentadien-1-ylidenebis(trimethyl-

Beteiligte Stoffe

Reaktionsbedingungen

Reaktionsschritte

14.7 g (0.106 moles) of trimethylsilylcyclopentadiene (obtained from Fluka) and 150 ml of tetrahydrofuran (THF) were placed in a reaction flask and cooled to 0° C. 47.4 ml of a solution of butyllithium in n-hexane (2.3 molar; total amount 0.109 moles) were added dropwise over 20 minutes. When the addition was complete, the yellow solution was stirred for a further one hour and the cooling bath was then removed. At room temperature the solution was stirred for a further one hour and then cooled to −20° C. 14.8 ml (0.117 moles) of trimethylsilyl chloride were then added dropwise over 10 minutes and the reaction mixture was stirred for two hours at −10° C. The cooling bath was then removed and the reaction solution was heated to room temperature and subsequently stirred for a further one hour. The reaction mixture was filtered through Celite; the filter was washed with hexane and the hexane was removed from the combined filtrates under vacuum. On distillation at 26° C. under 0.4 mbar, the crude product gave 19 g of pure compound 1 (85% of the theoretical yield). Boiling point and NMR data are consistent with the literature (J. Organometallic Chem. 29, (1971), 227; ibid. 30, (1971), C 57; J. Am. Chem. Soc. 102, (1980), 4429; J. Gen. Chem. USSR, Eng. Transl. 43, (1973), 1970; J. Chem. Soc., Dalton Trans. 1980, 1156). 1H NMR (400 MHz, C6D6): δ=6.74 (m, 2H); 6.43 (m, 2H); −0.04 (s, 18H).

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