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ChemicalBook CAS DataBase List BIS(METHYLDIMETHOXYSILYL)METHANE

BIS(METHYLDIMETHOXYSILYL)METHANE synthesis

4synthesis methods
-

Yield:18297-79-5 90%

Reaction Conditions:

in methanol at 25; for 4 h;Inert atmosphere;

Steps:

2.2.2

A three-necked flask equipped with a cooling condenser and a dropping funnel was dried at 60° C. under reduced pressure, and filled with nitrogen.The flask was charged with 59 g of sodium methoxide (compound 2) and 153 g of methanol. The mixture was stirred for 15 minutes at 300 rpm using a 3:1 motor. 86 g of bis(dichloromethylsilyl)methane (compound 1) obtained in the Synthesis Example 1 was then added dropwise over 2 hours using a dropping funnel, with the flask being kept in a water bath at 25° C. After the addition, the mixture was stirred for 2 hours. The sodium salt produced as a by-product was filtered using a glass filter covered with celite, and the salt was washed with 200 ml of hexane. The filtrate was concentrated using an evaporator under reduced pressure to obtain 100 g (yield: 90%) of bis(dimethoxymethylsilyl)methane (compound 3).The residual water content of the end product was 114 ppm. The content (metal impurity content) of elements other than silicon, carbon, oxygen, and hydrogen was as follows. Specifically, the Na content was 9 ppb, the K content was 6 ppb, the Fe content was 3 ppb, and the Ni content was 3 ppb. The content of each of Li, Fe, Cr, Ag, Cu, Zn, Mn, Co, Ti, Zr, Al, Pb, Sn, and W was equal to or less than the detection limit (0.2 ppb).

References:

US2011/82309,2011,A1 Location in patent:Page/Page column 4