2,3,3-三甲基哌啶

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 10 g of 4,4,-dimethyl-5-oxohexanenitrile (purity 97.2%) and 195 g of liquid ammonia were pumped hourly from bottom to top at 250 bar and 80° C. through a tubular reactor (diameter 16 mm, fill level 50 cm, oil-heated twin jacket) arranged before the hydrogenation reactor and filled with 63.5 g (100 ml) of titanium dioxide (anatase) in the form of 1.5 mm pellets. 100 l (s.t.p.)/h of hydrogen were subsequently passed in, and the product discharged from the upstream imination reactor was passed through the hydrogenation reactor from bottom to top at 250 bar and 110° C. The mixture was decompressed to atmospheric pressure, the ammonia was removed by distillation, and the hydrogenation product was analyzed quantitatively by means of gas chromatography, giving a yield of 93.0% of 4,4-dimethyl-1,5-hexanediamine and 4.5% of 2,3,3-trimethylpiperidine. to top at 250 bar and 80° C. through a tubular reactor (diameter 16 mm, fill level 50 cm, oil-heated twin jacket) to top at 250 bar and 110° C the ammonia was removed by distillation

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 10 g of 4,4,-dimethyl-5-oxohexanenitrile (purity 97.2%) and 195 g of liquid ammonia were pumped hourly from bottom to top at 250 bar and 80° C. through a tubular reactor (diameter 16 mm, fill level 50 cm, oil-heated twin jacket) arranged before the hydrogenation reactor and filled with 63.5 g (100 ml) of titanium dioxide (anatase) in the form of 1.5 mm pellets. 100 l (s.t.p.)/h of hydrogen were subsequently passed in, and the product discharged from the upstream imination reactor was passed through the hydrogenation reactor from bottom to top at 250 bar and 110° C. The mixture was decompressed to atmospheric pressure, the ammonia was removed by distillation, and the hydrogenation product was analyzed quantitatively by means of gas chromatography, giving a yield of 93.0% of 4,4-dimethyl-1,5-hexanediamine and 4.5% of 2,3,3-trimethylpiperidine. to top at 250 bar and 80° C. through a tubular reactor (diameter 16 mm, fill level 50 cm, oil-heated twin jacket) to top at 250 bar and 110° C the ammonia was removed by distillation