Fluorene → HCID 67259085, compound

Participants

Reaction Steps

A 2.5 M n-BuLi solution in hexane (16.75 mL, 41.88 mmol) was added dropwise at 0° C. under stirring to a solution of 6.63 g of fluorene (39.89 mmol) in 100 ml of Et2O in a 500 mL 3-necked round flask. The resulting orange solution was allowed to warm up to room temperature and stirred for 1.5 h. A solution of chloro(2,4,6-trimethyl-indenyl)dimethylsilane (10 g, 39.87 mmol) in 20 mL of THF was cooled to 0° C. and slowly added to the lithium salt solution, also previously cooled to 0° C. At the end of the addition a light brown suspension was obtained. The latter was allowed to warm up to room temperature and stirred for 1.5 h. Then the reaction mixture was evaporated under reduced pressure to give a brown sticky solid, which was treated at r.t. with 150 mL of toluene and then filtered to remove LiCl. The filtrate was dried in vacuo to give 16.42 g of a brown oil, which resulted to be the expected ligand contaminated by minor amounts of non identified by-products (crude yield quantitative). The product was used as such in the next step without further purification.

Provenance & Evidence