Sodium Acetate → 1-(Methoxydimethylsilyl)methanol 1-acetate

Temperature

150 °C

A mixture of 61.1 kg of Hydroseal G 400 H and 50 kg (609.4 mol) of sodium acetate was dried by heating at 150° C./2 mbar for 1 h. After cooling down to 112° C., the vacuum was broken with nitrogen, 3.76 kg (11.1 mol) of tetrabutylphosphonium bromide were added and the temperature was adjusted to 120° C. Then, under agitation, 76.8 kg (554 mol) of (chloromethyl)methoxydimethylsilane were metered in over 1 h. The mixture was subsequently stirred at the same temperature for a further 6 h. The product was then distilled out through a column at 20 mbar (head), 50-56° C. (head) and 70-145° C. (pot), while a further 36.7 kg of Hydroseal G 400 H were metered in during the distillation to ensure stirrability. The product (acetoxymethyl)methoxydimethylsilane (89.0 kg, 548.5 mol, 99% of theory; purity 99.5% (GC area %)) was obtained 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.

1. customwas dried
2. temperatureAfter cooling down to 112° C.
3. additionwere added
4. customwas adjusted to 120° C
5. customwere metered in over 1 h
6. distillationThe product was then distilled out through a column at 20 mbar (head), 50-56° C. (head) and 70-145° C. (pot), while a further 36.7 kg of Hydroseal G 400 H
7. distillationwere metered in during the distillation

ORD record

ord-322ccb67432443f4beb5a2738bf4097f

Source dataset

uspto-grants-2014_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08692012B2