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

Temperature

90 °C

A mixture of 230.4 kg (1.662 kmol) of (chloromethyl)-methoxydimethylsilane and 11.8 kg (34.8 mol) of tetrabutylphosphonium bromide was heated up to 90° C. and admixed during 3 h with 150 kg (1.828 kmol) of sodium acetate (anhydrous) in 6 portions of 25 kg each such that the temperature did not exceed 114° C. The mixture was subsequently stirred without additional heating for 1 h and then at 115-122° C. for a further 2 h. Thereafter, the product was distilled out through a column at 18-30 mbar (head), 50-53° C. (head) and 84-120° C. (pot), while 150 kg of Hydroseal G 400 H were metered into the residue during the distillation to ensure stirrability. The product (acetoxymethyl)methoxydimethylsilane (249.2 kg, 1.536 kmol, 92% of theory; purity 99.6% (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. customdid not exceed 114° C
2. temperaturewithout additional heating for 1 h
3. distillationThereafter, the product was distilled out through a column at 18-30 mbar (head), 50-53° C. (head) and 84-120° C. (pot), while 150 kg of Hydroseal G 400 H
4. distillationwere metered into the residue during the distillation

ORD record

ord-c95defa9233d494f989c5e4c57ad6d49

Source dataset

uspto-grants-2014_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08692012B2