Sodium Acetate → (Acetoxymethyl)dimethoxymethylsilane

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Reaction Steps

The top, Hydroseal phase and the middle, catalyst phase from Example 5b were admixed with 180 g (2.2 mol) of sodium acetate and the suspension was dried by distilling 10 mL of Hydroseal G 400 H off through a Vigreux column (80 cm) at 1-2 mbar (head), 120-135° C. (head), 150-160° C. (pot). The suspension was cooled down to 130° C., at which point 308 g (2.00 mol) of (chloromethyl)dimethoxymethylsilane were metered in over 47 minutes. The product was distilled out through a Vigreux column (80 cm); the product (acetoxymethyl)dimethoxymethylsilane was obtained at 30 mbar (head), 71-73° C. (head) and 73-80° C. (pot) in the distillate (334 g, 1.87 mol, 94% of theory; purity 99.1% (GC area %)) as a colorless liquid. The solvent, sodium chloride, excess sodium acetate and the phase transfer catalyst in the form of the chloride, bromide and acetate salt of tetrabutylphosphonium remained in the residue.

Provenance & Evidence