Silane, chloromethyl-trimethoxy- → (Trimethoxysilyl)methyl acetate

Temperature

120 °C

Example 2 was repeated using sodium acetate (312 g, 3.81 mol) and (chloromethyl)trimethoxysilane (563 g, 3.30 mol) as starting materials, tetrabutylphosphonium bromide (22.46 g, 66.2 mmol) as catalyst and methyl laurate (525 mL) as solvent. Before the silane was added, the other components were mixed and incipiently stripped at 116° C./4 mbar (for drying, 16 g of distillate). The silane was metered in at 120° C. over 2 hours, the mixture was heated at 120° C. for a further 4 hours and then distilled at 10-11 mbar (head), 74-76° C. (head) and 88-122° C. (pot) through a packed column (20 cm) to obtain 608 g (3.13 mol, 95% of theory) of (acetoxymethyl)trimethoxysilane in the distillate; purity 98.6% (GC area %). The solvent then started to pass over at 3.1 mbar (head), 113° C. (head) and 128° C. (pot). By distilling over a small amount (about 10 g) of the solvent, the product (acetoxymethyl)trimethoxysilane was fully removed from the residue. The remaining solvent, sodium chloride, excess sodium acetate and the phase transfer catalyst (in the form of the bromide, chloride and acetate salt of tetrabutylphosphonium) remained in the residue.

1. additionthe other components were mixed
2. customincipiently stripped at 116° C.
3. custom4 mbar (for drying, 16 g of distillate)
4. distillationdistilled at 10-11 mbar (head), 74-76° C. (head) and 88-122° C. (pot) through a packed column (20 cm)

ORD record

ord-56db9f19149b4eea9748f4e65679bfad

Source dataset

uspto-grants-2014_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08692012B2