Acetic Acid → Butyl prop-2-enoate--methyl 2-methylprop-2-enoate (1/1)

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Reaction Steps

A 2-liter flask was charged with 700 g of deionized water and 20 g of 1N acetic acid. While the flask was cooled with water so as to maintain the internal temperature below 30° C., with stirring, 544 g (4.0 mol) of methyltrimethoxysilane and 110 g (0.5 mol) of 3-glycidoxypropylmethyldimethoxysilane were added dropwise over 1-1/2 hours for hydrolysis. The reaction solution was ripened for 5 hours at 30° C. Methanol formed and water were distilled off at 60° C. and 30 mmHg in a total amount of 392 g. The reaction solution, which was cloudy at this point, was left to stand whereupon the silicone resin settled to the flask bottom. To this, 213 g of methyl methacrylate (MMA) and 142 g of butyl acrylate (BA) were added for dissolving the silicone resin again, obtaining 720 g of a MMA/BA solution of silicone resin. The solution was allowed to stand whereupon the aqueous layer separated off. To the organic layer, 72 g of 2-butoxyethyl acetate was added, obtaining a MMA/BA solution (A-7) (solids concentration 43.1%) of silicone resin (S-7). This silicone resin (S-7) is represented by the average compositional formula:

Provenance & Evidence