Pressionorm,Helopharm,W. Germany,1981
Hydrolysis of D-(+)-1-(3-rnethoxyphenyl)-2-aminopropane: 2.42 mols (40 g)
of the compound are dissolved in 6N hydrochloric acid in a bomb tube
consisting of stainless steel and having a capacity of 500 ml. Hydrogen
chloride gas is passed into the ice-cooled solution until this is saturated, The
solution is then heated to 130°C for 2 hours in an air bath. After cooling and
driving off the hydrochloric acid at a slightly elevated temperature, the
hydrochloride of the 3-hydroxyphenyl derivative is present in the form of a
yellowish syrup.
The free base can be liberated from the hydrochloride by extracting a butanol
solution of the hydrochloride several times with sodium bicarbonate solution.
After recrystallization from isopropanol/ligroin, the yield of D-(+)-1-(3-
hydroxyphenyl)-2-aminopropane amounts to 33.0 g, corresponding to 90.1%
of theory relative to the D-form. Melting point = 152°C to 154°C.
