[C:1]1([CH2:10][C:11]#[N:12])[CH:6]=[CH:5][CH:4]=[C:3]([CH2:7][C:8]#[N:9])[CH:2]=1.N>[Ni].C(O)C>[NH2:9][CH2:8][CH2:7][C:3]1[CH:4]=[CH:5][CH:6]=[C:1]([CH2:10][CH2:11][NH2:12])[CH:2]=1A mixture of 25.0 g (0.16 mmol) meta-xylylene dicyanide, 300 ml ethanol and50 ml conc. NH3 is hydrogenated in the presence of Raney nickel for 5 hrs. at 100° C. and 150 bar. One then filters off with suction and evaporates. The residue is dissolved in ether, the solution is clarified with active carbon and finally mixed with HCl-containing ether, whereby the dihydrochloride precipitates out. One filters off with suction, washeswith ether and dries. Yield 23.2 g (61% of theory) of dihydrochloride with the m.p. 282°-286° C.
Wird geladen…