3-[ethoxy(dimethyl)silyl]propane-1-thiol

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Added dropwise at 5° C., under argon, to 3-mercaptopropyldimethylethoxysilane (34.0 g, 0.191 mol) in solution in triethylamine (19.2 g, 0.191 mol) and cyclohexane (400 ml) is octanoyl chloride (31.0 g, 0.191 mol) over 15 minutes at 8° C. The reaction medium is stirred for 15 hours at ambient temperature. The precipitate of triethylamine hydrochloride Et3N.HCl is filtered. The mixture obtained is purified by flash chromatography (eluent: petroleum ether, 500-600 ml). After evaporating the solvents under reduced pressure at 24° C., the S-octanoylmercaptopropylethoxydimethylsilane E with CAS number [1024594-66-8] (45.0 g, 0.148 mol) is obtained in the form of a colourless liquid with a yield of 78%. over 15 minutes at 8° C The precipitate of triethylamine hydrochloride Et3N.HCl is filtered The mixture obtained is purified by flash chromatography (eluent: petroleum ether, 500-600 ml) After evaporating the solvents under reduced pressure at 24° C.

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Added, at ambient temperature, to a solution of S-(ethanoyl)mercaptopropylethoxydimethylsilane C (65.4 g, 0.297 mol) in absolute ethanol (230 ml) is solid sodium ethylate (2.02 g, 0.030 mol) under argon. The reaction medium is brought to reflux for 2.5 hours. After returning to ambient temperature, the precipitate of NaCl is filtered and washed with heptane (350 ml). After evaporating the solvents under reduced pressure at 45° C., the oil obtained is purified by vacuum distillation (60° C./10 mbar). The 3-mercaptopropylethoxydimethylsilane D with CAS number [141137-15-7] (34.7 g, 0.195 mol) is obtained with a yield of 66%. to reflux for 2.5 hours After returning to ambient temperature the precipitate of NaCl is filtered washed with heptane (350 ml) After evaporating the solvents under reduced pressure at 45° C. the oil obtained is purified by vacuum distillation (60° C./10 mbar)