Benzene, [dichloro(3-chloropropyl)silyl]- → 1-Chloro-1-phenylsiletane

Participants

Reaction Steps

A dry 1 L three neck round bottom flask equipped with a mechanical stirrer, dropping funnel, and condenser with nitrogen inlet system was charged with 18.3 g (0.75 mole) magnesium powder and 250 ml anhydrous diethyl ether. The magnesium was activated by the addition of 200 mg iodine. And then 50.7 g (0.20 mole)(3-chloropropyl)phenyldichlorosilane in 100 ml diethyl ether was added dropwise over 40 mins. at room temperature. The mixture was stirred for an additional 48 h and 200 ml anhydrous diethyl ether was added. The magnesium chloride and excess magnesium was filtered under nitrogen. The solid was washed with three portions of ether. The solvent was removed by the distillation and the product was distilled by reduced pressure. 22 g of 1-chloro-1-phenyl-1-silacyclobutane b.p. 83°-85° C./2 mm Hg was obtained.

Provenance & Evidence