反应详情

温度

70 °C

To a solution of 1,4-bis[5-(4-benzyloxy-3,5-dimethoxyphenyl)-2-pyridyl]hexahydro-1,4-diazepine (27.0 mg, 0.037 mmol) in methanol (1.0 mL) were added 10% palladium on charcoal (14.0 mg) and ammonium formate (14.0 mg, 0.220 mmol), and the resulting mixture was stirred at 70° C. for 2 hours. Insoluble materials were removed by filtration through Celite, and the filtrate was concentrated under reduced pressure. A solution of the residue in chloroform was washed with water and brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was recrystallized from methanol-chloroform-diethyl ether to yield the title compound as pale brown needles (melting point: 200.0–202.0° C.) (17.0 mg, yield: 85%).

1. customInsoluble materials were removed by filtration through Celite
2. concentrationthe filtrate was concentrated under reduced pressure
3. washA solution of the residue in chloroform was washed with water and brine
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe residue was recrystallized from methanol-chloroform-diethyl ether