Ammonia → 2-(3-Aminopropyl)-cyclohexylamine

Participants

Reaction Steps

Through a tubular reactor (diameter 16 mm, packing height 50 cm, oil-heated double jacket), installed up-stream of the hydrogenation reactor and packed with 70.0 g (100 g) of γ-aluminum oxide in he form of 1.5 mm extrudates, there were passed upwardly, per hour, 10.7 g of 2-(2-cyanoethyl)-cyclohexanone (purity 97.5%, 0.069 mole) and 500 ml of liquid ammonia (300 g, 17.6 moles) at a pressure of 250 bar and a temperature of 80° C. Hydrogen was then added to the stream at a rate of 60 standard liters (2.7 moles) per hour, and the effluent from the in-line imination reactor was passed upwardly through the hydrogenation reactor at a pressure of 250 bar and a temperature of 130° C. Gas-chromatographic analysis of the hydrogenation product gave 86.3% of 2-(3-aminopropyl)-cyclohexylamine and 7.9% of decahydroquinoline, corresponding to a yield of 2-(3-aminopropyl)-cyclohexylamine of 87.1% of theory.

Provenance & Evidence