Ammonia → Decahydroquinoline

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 64.4 g (92 ml) of γ-aluminum oxide there were passed upwardly, per hour, 55.4 g of 2-(2-cyanoethyl)-cyclohexanone (purity 96%, 0.352 mole) and 875 ml of liquid ammonia (525 g, 30.9 moles) at a pressure of 250 bar and a temperature of 70° C. Hydrogen was then added to the stream at a rate of 200 standard liters (8.9 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 120° C. After an on-stream of 3.5 hours the separation and distillation measures as per Example 2 had yielded, besides 33.1 g of decahydroquinoline, 138.8 of 2-(3-aminopropyl)-cyclohexylamine, this corresponding to a yield of 2-(3-aminopropyl)-cyclohexylamine of 71.5% of theory.

1. temperatureThrough a tubular reactor (diameter 16 mm, packing height 50 cm, oil-heated double jacket)
2. waitthere were passed upwardly, per hour
3. customa temperature of 70° C
4. customthe effluent from the in-line imination reactor was passed upwardly through the hydrogenation reactor at a pressure of 250 bar
5. customa temperature of 120° C
6. customAfter an on-stream of 3.5 hours the separation and distillation measures as per Example 2

ORDレコード

ord-7f0e252d87ca4f9e805d09549d82a4d2

出典データセット

uspto-grants-1993_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05239120