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ChemicalBook CAS DataBase List Dichloromethylsilane
75-54-7

Dichloromethylsilane synthesis

15synthesis methods
-

Yield:75-54-7 72.9 %Spectr. ,993-00-0 9.4 %Spectr.

Reaction Conditions:

with tetra-n-butylphosphonium chloride in diethylene glycol dimethyl ether at -196 - 120; for 19 h;Sealed tube;Temperature;

Steps:

2; 4 Example 1
General procedure: MeH2Si-SiH2Me (VIII, 0.8 mmol) and MeSiC (1.3 mmol) were mixed with a catalytic amount of the redistribution catalyst of n-Bu4PCI (0.02 mmol) in diglyme (0.35 ml) as solvent in an NMR tube, solidified at -196 °C (liquid nitrogen) and sealed in vacuo. After warming the samples to r.t.,29Si- and1H-NMR spectra were measured to prove the degree of SiH/SiCI redistributions after different reaction times and temperatures to control and quantify product formation by integration of the intensity of relevant NMR signals within the mixture. As displayed in Table 2 already after 14 h at 80 °C chlorosilane IV was nearly completely consumed to give nearly equimolar amounts of the target compounds V and VI (41 % vs. 42%). Taking the formation of hydridosilane VII (16%) into consideration, silicon-silicon bond cleavage, hydrogenation and subsequent redistribution reactions occurred quantitatively. Increasing the reaction temperature and time to 120 °C/42 h did not shift the redistribution equilibrium significantly. Table 2

References:

MOMENTIVE PERFORMANCE MATERIALS INC.;AUNER, Norbert;SANTOWSKI, Tobias;STURM, Alexander, G. WO2019/60486, 2019, A1 Location in patent:Page/Page column 41; 42

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