ethyl N-(3-triethoxysilylpropyl)carbamate

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

Procedure: In a 10 L distillation autoclave, 3-aminopropyltriethoxysilane (3321 g, 15 mol) are brought to reaction with urea (928 g, 15.45 mol) and ethanol (3458 g, 75 mol) at 230° C. and pressure between 35 and 23 bar. The resultant ammonia is continuously stripped out by the ethanol vapors.

Conditions: temp:-10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 3-Aminopropyltriethoxysilane (442 g.), light petroleum (b.p. 30°-40°, 1600 ml) and anhydrous triethylamine (255 g.) were placed under dry nitrogen in a three-necked flask equipped with a stirrer and dropping funnel. The mixture was cooled to -10° C. and a solution of redistilled ethyl chloroformate (217 g.) in light petroleum (b.p. 30°-40° C., 600 ml) was added dropwise over 2 h. The mixture was allowed to warm to ambient temperature and left overnight. The mixture was then rapidly filtered and the solid washed with light petroleum (2 × 300 ml). The combined filtrate was then concentrated and fractionally distilled to give ethyl-N-(3-triethoxysilylpropyl)carbamate (517 g.), b.p. 125°-135° C./0.09 mm. equipped with a stirrer to warm to ambient temperature The mixture was then rapidly filtered the solid washed with light petroleum (2 × 300 ml) The combined filtrate was then concentrated fractionally distilled