Welcome to LookChem.com Sign In | Join Free

Details

Home > Chemical Encyclopedia > Chemical Technology > Organic Chemical Technology >
 Production Method of Tris(trimethylsilyl)silane
  • Production Method of Tris(trimethylsilyl)silane
  • (trimethylsilyl)silane (CAS NO.: ), which is also known as Trisilane, 1,1,1,3,3,3-hexamethyl-2-(trimethylsilyl)-, could be produced through the following synthetic routes.

    Production Method of Tris(trimethylsilyl)silane

    powder (7.55 g, 1.07 mol) is placed in a 500-mL, four-necked flask equipped with a condenser, mechanical stirrer, dropping funnel, and low-temperature thermometer. The apparatus is carefully flushed several times with nitrogen followed by the addition of 50 mL of anhydrous tetrahydrofuran (THF). The reaction flask is cooled to approximately -60°C in a dry ice-acetone bath, and a mixture of freshly distilled (from CaH2) chlorotrimethylsilane (54.8 mL, 47.1 g, 0.43 mol) and tetrachlorosilane (10.1 mL, 15.0 g, 0.09 mol) in 140 mL of anhydrous THF is added over 1 hr by dropping funnel so that the temperature of the reaction mixture never exceeds -30°C. After addition is complete, stirring is continued for 0.5 hr with cooling. The gold-brown suspension is allowed to warm to room temperature and stirred for 12 hr, during which time the color becomes more intense. The thermometer is removed and the mixture is heated to reflux for 2 hr to destroy the remaining chlorotrimethylsilane. After the condenser is cooled to room temperature, it is replaced with a nitrogen bubbler and gas inlet. Methyllithium-lithium bromide complex (66 mL, 99 mmol, 1.5 M in ether) is added over 3 hr to the grey-brown mixture with vigorous stirring. During the addition a continuous stream of nitrogen is bubbled through the reaction mixture. After the reaction mixture is stirred for an additional 16 hr at room temperature, it acquires a greenish tint. Hydrolysis is carried out by the careful addition of the reaction mixture to 400 mL of ice-cold 2 N hydrochloric acid. [CAUTION: The solid residue may be highly pyrophoric. The checkers blanketed the flask with argon prior to the introduction of ether (100 mL) and poured the vigorously stirred slurry into the cold hydrochloric acid. This rinse procedure was repeated twice more.] The aqueous phase is extracted four times with 200-mL portions of pentane, the combined organic phases are dried over magnesium sulfate and the solvents removed under reduced pressure. Distillation under reduced pressure (1 mm, 38°C) affords 13.4–17.2 g of the product as a clear oil (60–77% yield).


    Prev:No record
    Next:No record
  • Back】【Close 】【Print】【Add to favorite
Periodic Table
    Hot Products