Dichlorodimethylsilane → HCID 59735669, compound

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Reaction Steps

A 2.5 M n-BuLi solution in hexane (37.2 mL, 0.093 mol) was added dropwise at 0° C. under nitrogen atmosphere to a solution of 14.00 g of 2,4,6-trimethyl-indene (prepared according to Eur. Pat. Appl. 693,506) in 100 mL of Et2O in a 500 mL 3-necked round flask. During the addition a white suspension was formed. The mixture was then allowed to warm up to r.t. and stirred for 30 min, with final formation of a white suspension. Then a solution of Me2SiCl2 (98%, d=1,064, 11.28 mL, 0.093 mol.) in 30 mL of THF was cooled to 0° C. and slowly added to the lithium salt suspension, also cooled to 0° C. The reaction mixture was allowed to warm up to r.t. and stirred for 2 h with final formation of a light yellow suspension. The solvents were then removed in vacuo and the residue was extracted with 150 mL of toluene to remove the LiCl. The light yellow filtrate was brought to dryness in vacuo to give 21.53 g of a yellow oil, characterized by 1NMR analysis as the target product, yield 97.5%. This product was used as such in the next step without further purification.

Provenance & Evidence