反应详情

A solution of 3-chloro-pyridine 1-oxide (2.40 g, 18.5 mmol) in piperidine (6 mL) was heated at 140° C. for 2 days. After the reaction mixture was cooled to room temperature the amine was removed, and the residue was purified by flash chromatography on a silica gel column (6:1 EtOAc/MeOH), affording 3,4,5,6-tetrahydro-2H-[1,3′]bipyridinyl 1′-oxide as a pale yellow solid (2.20 g, 67%). 1H NMR (CDCl3) δ 1.59-1.67 (m, 6H), 3.14-3.18 (m, 4H), 6.78 (dd, 1H, J=2.1, 8.7 Hz), 7.03 (dd, 1H, J=6.3, 8.7 Hz), 7.63-7.66 (m, 1H), 7.85-7.86 (m, 1H).

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2. customthe residue was purified by flash chromatography on a silica gel column (6:1 EtOAc/MeOH)