反应详情

温度

80 °C

To a pyridine solution (0.5 mL) of 5-(4-aminophenyl)-1,5,8,9,10,11-hexahydronaphtho[1,2-b][1,4]diazepine-2,4-dione (20 mg, 0.062 mmol) obtained in Example 10 was added isobutyryl chloride (10 μL, 0.093 mmol). The mixture was stirred at 80° C. for 1 hour. To the reaction mixture was added aqueous solution of hydrochloric acid under cooling in ice-bath. The mixture was stirred for 20 minutes. Insoluble was collected by filtration, and washed with water. The residue was purified by silica gel column chromatography (chloroform/methanol=99/1) to give the titled compound as white powder (23 mg, yield 95%).

1. temperatureunder cooling in ice-bath
2. stirringThe mixture was stirred for 20 minutes
3. filtrationInsoluble was collected by filtration
4. washwashed with water
5. customThe residue was purified by silica gel column chromatography (chloroform/methanol=99/1)