Silane → (Acetoxymethyl)dimethoxymethylsilane

Temperatur

150 °C

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).

1. custom2 mbar (for drying)
2. additionwere added
3. customwas adjusted to 120° C
4. customwere metered in over 2 hours
5. distillationThe product was distilled out through a sieve plate column

ORD-Eintrag

ord-2599a226ef8d4e4890a51c26d26b1377

Quelldatensatz

uspto-grants-2014_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08692012B2