反应详情

41.6 g per hour of 2-butyl-2-ethyl-4-cyanobutanal (purity 90%, 37.4 g, 0.207 mol) and 1073 ml (646 g, 38.0 mol) per hour of liquid ammonia were pumped at 250 bar and 50° C. through a tubular reactor (diameter 16 mm, fill level 50 cm, oil-heated twin jacket) upstream of the hydrogenation reactor and filled with 43.3 g (96 ml) of a Y-zeolite pelleted with Aerosil 200 (HY-zeolite: Aerosil 200 =9:1, SiO2 :Al2O3 =6:1). The product stream was subsequently passed through the hydrogenation reactor from bottom to top at 250 bar and 120° C. while simultaneously passing 80 l(S.T.P.)/h (3.6 mol) of hydrogen through the reactor. The product stream was decompressed to atmospheric pressure and NH3 was removed by distillation. The product from 34.1 hours was separated by fractional distillation on a 30 cm packed column (3 mm glass rings), giving 358.3 g of 3-butyl-3-ethylpiperidine and 747.7 g of 2-butyl-2-ethylpentane-1,5-diamine. The diamine yield was 56.9% of theory.

1. temperature(diameter 16 mm, fill level 50 cm, oil-heated twin jacket) upstream of the hydrogenation reactor
2. customto top at 250 bar and 120° C.
3. customwas removed by distillation
4. customThe product from 34.1 hours was separated by fractional distillation on a 30 cm