Manufacturing Process
1) 28.05 g of 2-phenyl-3-aminobicyclo[2.2.1]heptane are mixed with 6.9 g
acetaldehyde keeping the mixture cool. The mixture is heated for 20 minutes
on the stream bath under reflux, and the reaction product is freed from water
in vacuum at 60°C. The crude base is dissolved in 300 ml of methanol and
hydrogenated with 2 previously reduced platinum oxide. After it has taken up
the calculated quantity of hydrogen, the solvent is distilled off in vacuum, the
residue dissolved in dilute hydrochloric acid and the neutral by-products are
shaken out with ether. The aqueous solution is made alkaline with caustic
soda and extracted with ether. From ethereal solution 13.2 g of the base are
obtained with a boiling point at 1 mm of 128°-131°C.
25 g of 2-phenyl-3-aminobicyclo[2.2.1]heptane,15 g Raney nickel and 75
ml absolute alcohol are boiled under a reflux for 15 hours. The filtrate from
the catalyst is neutralised with dilute hydrochloric acid and distilled to dryness
in vacuum. The hydrochloric residue is purified by recrystallisation from
acetone or dioxane-petrol-ether. Yield 21.5 g; MP: 191°C.
