Silane → (Acetoxymethyl)dimethoxymethylsilane

関与物質

反応条件

反応手順

A mixture of 10.7 L of Hydroseal G 400 H(═HSB, C17-C21 hydrocarbon mixture, see above) and 5.97 kg (72.8 mol) of sodium acetate was heated up for one hour at 150° C./2 mbar (for drying). The heating was switched off, the vacuum was broken with nitrogen and 450 g (1.32 mol) of tetrabutylphosphonium bromide (=phase transfer catalyst) were added and the temperature was adjusted to 120° C. Under agitation, 10.24 kg (66.2 mol) of (chloromethyl)dimethoxymethylsilane (=a silane of formula II) were metered in over 2 hours. The mixture was stirred at the same temperature for a further 3 hours. The product was distilled out through a sieve plate column; the product (acetoxymethyl)dimethoxymethylsilane was obtained at 53-54 mbar (head), 70-73° C. (head) and 100-125° C. (pot) in the distillate (10.8 kg, 60.6 mol, 92% of theory; purity 99.5% (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 (18.5 kg in total).

情報源と証拠