6-(AMINOMETHYL)-3-AMINOPYRIDINE synthesis

Yield:771574-03-9 57%

Reaction Conditions:

with ammonia;hydrogen;Raney nickel in methanol at 20; for 24 h;

Steps:

13

1.24 g (96 percent, 10.0 mmol) 5-amino-2-cyanopyridine in methanolic ammonia solution were hydrogenated at 5 bar hydrogen pressure and ambient temperature for 24 h through Raney nickel. Then the catalyst was separated off, and the mixture was filtered through silica gel. 500 mg of the residue remaining after evaporation were stirred with dichloromethane. Then 4-molar hydrogen chloride/dioxane mixture was added and stirred for 14 h. The resulting solid was suction filtered and dried.Yield: 750 mg (57%).ES-MS (M+H)⁺=124RT (HPLC-MS)=0.73 min

References:

US2010/144681,2010,A1 Location in patent:Page/Page column 102