反应详情

80.0 g per hour of 2-butyl-2-ethyl-4-cyanobutanal (purity 99.3%, 0.44 mol) and 200 g (330 ml, 11.76 mol) per hour of liquid ammonia were pumped from bottom to top at 250 bar and 80° C. through a tubular reactor (diameter 16 mm, fill level 20 cm, oil-heated twin jacket) upstream of the hydrogenation reactor and filled with 25.4 g (40 ml) of TiO2 (anatase) in the form of 1.5 mm pellets. 100 l(S.T.P.)/h of hydrogen were then fed in, and the product stream from the upstream imination reactor was passed through the hydrogenation reactor from bottom to top at 250 bar and 110° C. The product stream was decompressed to atmospheric pressure and the ammonia was removed by distillation. According to gas-chromatographic analysis, the hydrogenation product stream contained 89.2% of 2-butyl-2-ethylpentane-1,5-diamine and 4.3% of 3-butyl-3-ethylpiperidine. The product from 80.5 hours was separated by fractional distillation on a 30 cm packed column (3 mm glass rings), giving 5738 g of 2-butyl-2-ethylpentane-1,5-diamine, corresponding to a yield of 87.3% of theory.

1. customto top at 250 bar and 80° C. through a tubular reactor
2. temperature(diameter 16 mm, fill level 20 cm, oil-heated twin jacket) upstream of the hydrogenation reactor
3. customto top at 250 bar and 110° C
4. customthe ammonia was removed by distillation
5. customThe product from 80.5 hours was separated by fractional distillation on a 30 cm