反应详情

To a solution of 1,4-bis[5-(3,4,5-triethoxylphenyl)-2-pyridyl]hexahydro-1,4-diazepine (77 mg, 0.115 mmol) in methanol (5.0 mL) was added a 1.0 M aqueous methanesulfonic acid (0.23 mL, 0.23 mmol), and the reaction mixture was concentrated under reduced pressure. Ethanol (5.0 mL) was added to the residue, and the resulting mixture was concentrated under reduced pressure. The residue was recrystallized from methanol-diethyl ether to yield the title compound as a pale yellow crystalline powder (melting point: 235.0–237.0° C.) (74.0 mg, yield: 94%).

1. concentrationthe reaction mixture was concentrated under reduced pressure
2. additionEthanol (5.0 mL) was added to the residue
3. concentrationthe resulting mixture was concentrated under reduced pressure
4. customThe residue was recrystallized from methanol-diethyl ether