反应详情

To a mixture of 1-methyl-2-[1-(4-piperazin-1-ylmethyl-phenyl)piperidin-4-yloxy]-1H-[4,4′]bipyrimidinyl-6-one (80 mg, 0.17 mmol), formaldehyde solution (37% in water, 55 mg, 0.68 mmol) and acetic acid (one drop) in 1,2-dichloroethane (0.85 ml) was added sodium triacetoxyborohydride (130 mg, 0.61 mmol). The mixture was stirred at room temperature for 2 hours. The mixture was partitioned between water and chloroform. The organic layer was dried over sodium sulfate, and concentrated in vacuo. The residue was purified by silica gel column chromatography (eluent; chloroform/methanol=95/5) to afford 1-methyl-2-{1-[4-(4-methyl-piperazin-1-ylmethyl)phenyl]piperidin-4-yloxy}-1H-[4,4′]bipyrimidinyl-6-one as a colorless solid (49 mg, 0.10 mmol, 59%)

1. customThe mixture was partitioned between water and chloroform
2. dry with materialThe organic layer was dried over sodium sulfate
3. concentrationconcentrated in vacuo
4. customThe residue was purified by silica gel column chromatography (eluent; chloroform/methanol=95/5)