反应详情

温度

50 °C

To a solution of 1,4-bis[5-(4-benzyloxycarbonylamino-3,5-dimethoxyphenyl)-2-pyridyl]hexahydro-1,4-diazepine (120.0 mg, 0.140 mmol) in acetic acid (2.0 mL) was added 10% palladium on charcoal (24.0 mg), and the resulting mixture was stirred at 50° C. for 1.5 hours under hydrogen. 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 saturated aqueous sodium hydrogencarbonate and brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. To a solution of the residue in chloroform (5.0 mL) a 4.0 M solution of hydrogen chloride in ethyl acetate (0.14 mL, 0.56 mmol), and the resulting mixture was concentrated under reduced pressure. Ethanol (5.0 mL) was added to the residue, and the resulting mixture was concentrated under reduced pressure. Diethyl ether was added to the residue, and the resulting precipitate was collected by filtration to yield the title compound as a pale brown amorphous powder (84.0 mg, yield: 82%).

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 saturated aqueous sodium hydrogencarbonate and brine
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationconcentrated under reduced pressure
6. concentrationthe resulting mixture was concentrated under reduced pressure
7. additionDiethyl ether was added to the residue
8. filtrationthe resulting precipitate was collected by filtration