反应详情

A solution of 1,1-dimethylethyl 4-{[(5-chloro-6-methyl-3-pyridinyl)methyl]amino}-1-piperidinecarboxylate (65.58 g, 193 mmol) in DCM (800 ml) at 0° C. was treated with HCl (4M solution in 1,4-dioxane, 386 ml, 1544 mmol) and stirred at room temperature overnight. The resulting white suspension was filtered, washed with DCM and hexane and dried to obtain N-[(5-chloro-6-methyl-3-pyridinyl)methyl]-4-piperidinamine dihydrochloride (62.3 g) as a white solid. The crude product was dissolved in DCM/MeOH 5% (800 ml) and 2N NaOH (500 ml) was added until pH 13.8. Organic phase was extracted and aqueous phase was extracted again with DCM/MeOH 10% (650 ml×2). Combined organic phases were washed with brine, dried (MgSO4), filtered and concentrated under vacuum to give N-[(5-chloro-6-methyl-3-pyridinyl)methyl]-4-piperidinamine (44.82 g, 97%).

1. filtrationThe resulting white suspension was filtered
2. washwashed with DCM and hexane
3. customdried