Method for producing phosphonate-modified silicones
A phosphonate and organosiloxane technology, applied in the field of organosilicon compounds, can solve the problems of reduced reactive group concentration, slow reaction, undesired by-products of yield loss and the like
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Embodiment 1
[0062] Embodiment 1 (not the present invention):
[0063] In a 250 ml three-necked pouring flask with a dropping funnel and a reflux condenser, precharge 99.7 g (0.6 mol) of triethyl phosphite (P(OEt) 3 , Aldrich, GC 98%). After heating to 140° C., 46.4 g (0.3 mol) of chloromethyldimethoxymethylsilane (Wacker Chemie GmbH, Munich) were slowly added dropwise within 3 hours under vigorous stirring. Subsequently, the reaction mixture was continued to be heated to 170° C. for 30 minutes. After removing the excess triethyl phosphite in vacuo, 58.6 g of phosphodiethoxycarboethoxymethyldimethoxymethylsilane (0.23 mol , GC 98%, yield: 76% of theory).
Embodiment 2
[0064] Embodiment 2 (not the present invention):
[0065] In a 250 ml three-necked pouring flask with a dropping funnel and a reflux condenser, precharge 124.5 g (0.75 moles) of triethyl phosphite (P(OEt) 3 , Aldrich, GC 98%). After heating to 140° C., 69.3 g (0.5 mol) of chloromethyldimethylmethoxysilane (Wacker Chemie GmbH, Munich) were slowly added dropwise over 2.5 hours with vigorous stirring. Subsequently, the reaction mixture was continued to be heated to 170° C. for 30 minutes. After removal of excess triethyl phosphite in vacuo, 100.4 g of phosphodiethoxycarboethoxymethyldimethylmethoxysilane ( 0.42 mol, GC 98.2%, yield: 83.6% of theory).
Embodiment 3
[0066] Embodiment 3 (not the present invention):
[0067] In a 250 ml three-necked pouring flask with a dropping funnel and a reflux condenser, precharge 112.2 g (0.675 moles) of triethyl phosphite (P(OEt) 3 , Aldrich, GC98%). After heating to 140° C., 76.8 g (0.45 mol) of chloromethyltrimethoxysilane (Wacker Chemie GmbH, Munich) were slowly added dropwise over 2.5 hours with vigorous stirring. Subsequently, the reaction mixture was continued to be heated to 170° C. for 30 minutes. After removal of excess triethyl phosphite in vacuo, 105.6 g of phosphodiethoxycarboethoxymethyltrimethoxysilane (0.39 mol, GC 97.4%, yield: 86.2% of theory).
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Abstract
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