Lithium, ferrocenyl-(8CI,9CI) synthesis

9synthesis methods

Product Name:Lithium, ferrocenyl-(8CI,9CI)
CAS Number:1271-15-4
Molecular formula:C10FeLi
Molecular Weight:182.9

102-54-5 Synthesis

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Yield:1271-15-4 59%

Reaction Conditions:

in tetrahydrofuran;hexane at -78 - 0;Inert atmosphere;

Steps:

General procedures

^tBuLi (45 mL of a 1.6 M solution in hexanes, 72 mmol) was added over 15 min to a suspension of ferrocene (16.0 g, 86 mmol) in THF (80 mL) at 0 °C.
Immediately after the addition of t-BuLi, hexane (150 mL) was added and the suspension cooled to -78 °C.
The resulting pyrophoric orange precipitate was separated by filtration at -78 °C, washed with pre-cooled hexane (4 * 50 mL) at -78 °C and volatiles removed in vacuo to afford an orange powder (approximately 15 g).
This powder was continuously extracted with hexane (200 mL) using a Soxhlet apparatus over a period of 12 h, until the extracts were colourless.
The remaining solid was dried in vacuo to afford the target material as a highly pyrophoric orange powder.
Yield 8.17 g, 59%.

References:

Kelly, Michael J.;Tirfoin, Remi;Gilbert, Jessica;Aldridge, Simon [Journal of Organometallic Chemistry,2014,vol. 769,p. 11 - 16]