Silane → 1-(Methoxydimethylsilyl)methanol 1-acetate

A mixture of 20 mL of high boiler solvent as per Table 1, 13.5 g (165 mmol) of sodium acetate (anhydrous) and the Table 1 amount of phase transfer catalyst (amount specified in mol % based on employed amount of silane) was heated to the temperature reported in Table 1 and dried at this temperature under a vacuum of 10 mbar for minutes. The vacuum was subsequently broken with argon, and (chloromethyl)methoxydimethylsilane (20.8 g, 150 mmol) was metered in at this temperature over 30 minutes under agitation. The mixture was further stirred at this temperature until a gas chromatogram (FID detector) or a 1H NMR spectrum indicated more than 99% conversion of the silane; the reaction times required for this are reported in Table 1. The product was subsequently distilled off at 10-90 mbar (head), 50-90° C. (head) and 70-120° C. (pot) through a Widmer column (20 cm) to obtain the Table 1 yields of (acetoxymethyl)methoxydimethylsilane as a colorless liquid having a purity of >99% (GC area %). The solvent, sodium chloride, excess sodium acetate and the phase transfer catalyst in the form of its chloride and acetate salts (and also of the bromide salt when a bromide was used) remained in the residue.

1. customdried at this temperature under a vacuum of 10 mbar for minutes
2. customthe reaction times
3. distillationThe product was subsequently distilled off at 10-90 mbar (head), 50-90° C. (head) and 70-120° C. (pot) through a Widmer column (20 cm)
4. customto obtain the Table 1

ORDレコード

ord-768319b7d1d54b0f8968233ad8c26ab4

出典データセット

uspto-grants-2014_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08692012B2