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ChemicalBook CAS DataBase List CHLOROPHENYLSILANE 97

CHLOROPHENYLSILANE 97 synthesis

12synthesis methods
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Yield: 38% , 33% , 19%

Reaction Conditions:

with sodium hydride;lithium chloride in diethylene glycol dimethyl ether at 160; for 14 h;Inert atmosphere;

Steps:

13 Synthesis of phenylsilane (PhSiH3), phenylchlorosilane (PhSiH2CI) and phenyldichlorosilane (PhSiHCI2) by reduction of PhSiCl3 with the LiCI/NaH reagent
In a 500 ml three-necked flask equipped with a dropping funnel, reflux condenser, thermometer and a magnetic stirrer were placed 5.41 g (0.13 mol) LiCI and 24.10 g(1.00 mol) NaH, suspended in 100 ml of thoroughly dried diglyme. The LiCI/NaH/diglyme suspension was carefully scaled from oxygen/air by degassing the suspension in vacuo and refilling with gaseous nitrogen to establish inert conditions. PhSiCl3 (60.44 g, 0.29 mol) was slowly added over the dropping funnel and the reaction started upon heating the mixture to 160 °C with formation of solid NaCI. After 14 h reaction time the product mixture wasanalyzed by NMR spectroscopy, which revealed a product distribution of 38 % PhSiH2CI (15.40 g, 0.11 mol), 33 % PhSiHCI2 (16.60 g, 0.09 mol) and 19 % PhSiH3 (5.84 g, 0.05 mol); 10 % of PhSiCl3 (6.00 g, 0.03 mol) remained unreacted.

References:

MOMENTIVE PERFORMANCE MATERIALS INC.;AUNER, Norbert;SANTOWSKI, Tobias;STURM, Alexander, G. WO2019/60475, 2019, A2 Location in patent:Page/Page column 47

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