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ChemicalBook CAS DataBase List TRIMETHYLSILANE

TRIMETHYLSILANE synthesis

13synthesis methods
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Yield:993-07-7 92%

Reaction Conditions:

with lithium aluminium tetrahydride;calcium hydride in diethylene glycol dimethyl ether for 11 h;Inert atmosphere;Reflux;

Steps:

14
The 100 mL three-neck round bottom flask was dried, connected to a mechanical stirrer, a spherical condenser, a constant pressure funnel and a gas guiding device, and the spherical condensation tube tail gas was connected to a dry ice trap device to receive a low boiling point product.The nitrogen was then replaced by vacuum three times while the hot air gun was baked to remove the attached moisture.Under a nitrogen atmosphere,4.65 g (0.11 mol) CaH2, 0.38 g was added to the reaction flask.(0.01 mol) lithium aluminum hydride, 25 mL diethylene glycol dibutyl ether solvent.After heating to 55 ° C for 1 hour mechanical stirring,21.7 g (0.2 mol) of Me3SiCl in a constant pressure funnel was slowly added dropwise to the reaction flask, and after the completion of the dropwise addition, the reflux reaction was continued at 55 ° C for 10 hours.The main reduction product obtained was Me3SiH, and the reaction yield was 92%.

References:

Chinese Academy Of Sciences Chemical Institute;Li Yongming;Chen Yi;Xu Caihong;Wang Xinliang CN108285467, 2018, A Location in patent:Paragraph 0092-0093

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