trimethyl-(2-phenyl-1-trimethylsilyloxyethenoxy)silane

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution of butyllithium in hexane (0.4 mol, 250 ml of 1.6 M solution) was added to a solution of 40 g (0.4 mol) of diisopropylamine in 300 ml of tetrahydrofuran cooled in an ice-bath. A solution of 27.23 g (0.2 mol) of benzeneacetic acid in 200 ml of tetrahydrofuran was added near 0° C. and the reaction mixture was stirred for 30 minutes at 0° C. A 100 g portion of trimethylchlorosilane was added, the mixture was warmed to room temperature, stirred for 1.5 hours, and then filtered under nitrogen. The filtrate was evaporated to dryness under reduced pressure; the residue was dissolved in 80 ml of diethyl ether and filtered. The filtrate was evaporated to dryness and then distilled to give 37.2 g of β,β-[bis(trimethylsiloxy]styrene as a colorless liquid: bp 95° C. (0.5 mm). cooled in an ice-bath the mixture was warmed to room temperature stirred for 1.5 hours filtered under nitrogen The filtrate was evaporated to dryness under reduced pressure the residue was dissolved in 80 ml of diethyl ether filtered The filtrate was evaporated to dryness distilled