Ammonia → 4,4-Dimethyl-1,5-hexanediamine

Participants

Reaction Steps

21 g of 4,4-dimethyl-5-oxohexanenitrile (purity 97.2%) and 180 g of liquid ammonia were pumped hourly from bottom to top at 250 bar and 80° C. through a tubular reactor (diameter 0.16 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 at atmospheric pressure, and the ammonia was removed by distillation. The discharge from 24 hours was separated by fractional distillation on a 30 cm packed column (3-mm glass rings). 445 g of 4,4-dimethyl-1,5-hexanediamine were obtained as a colorless liquid (b.p. 90° C./3 mbar), corresponding to a yield of 88%.

Provenance & Evidence