Bis(eta-cyclopentadienyl) iron → HCID 129792804, compound

Participants

Reaction Steps

Ferrocene, 7.44 g (0.040 mole), and 1,6-dioxaspiro-[4,4]-nonane (I), 1.28 g (0.010 mole), were dissolved in 100 ml of methylene chloride and 3.6 ml (0.03 mole) of boron trifluoride etherate [BF3 . 0(Et)2 ] was added with stirring. After 2 hours of stirring, the reaction mixture was poured onto a dry alumina column (5 cm by 25 cm). Unreacted ferrocene, 6.3 g, was eluted from the column using ethylene dichloride. The chromatogram was then developed with a 1 to 1 mixture of ether (ethyl) and ethylacetate. The principal band (middle portion of the column) was cut out and extracted with methyl alcohol to give 1.72 g (55% yield) of II, mp 50°-53°C, after recrystallization from a 1 to 1 mixture of pentane and cyclohexane.

Provenance & Evidence