Sodium Acetate → (Acetoxymethyl)dimethoxymethylsilane

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.

1. customthe suspension was dried
2. distillationby 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)
3. customwere metered in over 47 minutes
4. distillationThe product was distilled out through a Vigreux column (80 cm)

ORDレコード

ord-c37541d8f94f4631a7cd70004a42acb6

出典データセット

uspto-grants-2014_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08692012B2