3-triethoxysilylpropanenitrile

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: Utilizing a 15 gallon high pressure stainless steel system, 80 pounds of beta-cyanoethyltriethoxysilane and 8 pounds of diethylamine were added initially. With a diptube, 12 pounds of hydrogen sulfide was charged into the reactor while cooling was maintained. The reactor was then heated to 60° C. with stirring for 6 hours. The residual hydrogen sulfide (80 psig) was carefully vented into a caustic scrubber and the product thioamide (94 pounds) was collected. The product, analyzed by InfraRed Spectroscopy, contained 5% unreacted nitrile. were added initially while cooling was maintained the product thioamide (94 pounds) was collected

Conditions: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: Into a clean, dry 300 milliliter high pressure reaction vessel was added 200 grams (0.92 moles) of beta-cyanoethyltriethoxysilane and 10 grams of diethylamine. The reactor was cooled to the temperature of solid carbon dioxide, and 42.0 grams (1.3 moles) of hydrogen sulfide was added via a calibrated metering system. The reactor was placed in a rocker and with agitation was heated to 60° C. for 5 hours. The pressure of the system increased to a maximum of 140 psig and decreased to 70 psig when the reaction was terminated. The final pressure at ambient temperature was 30 psig. The yield of crude beta-triethoxysilylthiopropionamide product was 258.4 grams. Analysis of the product mixture indicated 19 mg/g or 16% unreacted beta-cyanoethyltriethoxysilane. Into a clean, dry 300 milliliter high pressure reaction vessel was added via a calibrated metering system The pressure of the system increased to a maximum of 140 psig was terminated at ambient temperature