反应详情

To a solution of 4-(4-{2-[bis-(4-methoxy-benzyl)-amino]-pyrimidin-5-yl}-2-morpholin-4-yl-5,6-dihydro-pyrrolo[2,3-d]pyrimidin-7-yl)-benzaldehyde (76 mg, 0.118 mmol) in dichloromethane (2 ml), 1-methylpiperazine (40 μl, 0.354 mmol), sodium triacetoxy borohydride (100 mg, 472 mmol) and acetic acid (12.6 μl, 0.236 mmol) were added, followed by stirring at room temperature for 40 hours. To the reaction mixture, saturated aqueous ammonium chloride solution was added, followed by extraction twice with ethyl acetate (10 ml). The organic layer was washed with brine (10 ml), and dried over sodium sulfate, followed by distilling off under reduced pressure, and the resulting residue was purified by silica gel column chromatography (dichloromethane/2M-ammonia methanol=100/1 to 30/1), whereby bis-(4-methoxy-benzyl)-(5-{7-[4-(4-methyl-piperazin-1-ylmethyl)-phenyl]-2-morpholin-4-yl-6,7-dihydro-5H-pyrrolo[2,3-d]pyrimidin-4-yl}-pyrimidin-2-yl)-amine was obtained as a brown powder (44 mg, 51%).

1. extractionfollowed by extraction twice with ethyl acetate (10 ml)
2. washThe organic layer was washed with brine (10 ml)
3. dry with materialdried over sodium sulfate
4. distillationby distilling off under reduced pressure
5. customthe resulting residue was purified by silica gel column chromatography (dichloromethane/2M-ammonia methanol=100/1 to 30/1)