Ammonia → 2-Methyl-2-propylpentane-1,5-diamine

Participants

Reaction Steps

Example 3 was repeated, with 78.5 g per hour of 2-methyl-2-propyl-4-cyanobutanal (purity 86.6%, 68.0 g, 0.444 mol) and 1340 ml (804 g, 47.3 mol) per hour of liquid ammonia at 250 bar and 60° C. being pumped through the imination reactor. The product stream was subsequently passed through the hydrogenation reactor from bottom to top at 250 bar and 120° C. while simultaneously passing 150 l(S.T.P.)/h (6.7 mol) of hydrogen through the reactor. The product stream was decompressed to atmospheric pressure and NH: was removed by distillation. The product from 4.2 hours was separated by fractional distillation on a 30 cm packed column (3 mm glass rings), giving 96.0 g of 3-methyl-3-propylpiperidine and 162.8 g of 2-methyl-2-propylpentane-1,5-diamine. The diamine yield was 55.1% of theory.

Provenance & Evidence