反应详情

温度

60 °C

To a solution of hydroxylamine hydrochloride (4.34 g, 62.4 mmol) and N-ethyl-N-isopropylpropan-2-amine (12.7 mL, 72.8 mmol) in methanol (70 mL)/ethanol (70 mL) was added ethyl{[(5-{3-[(tert-butoxycarbonyl)amino]phenoxy}pyridin-2-yl)amino]carbonothioyl}carbamate (4.50 g, 10.4 mmol), and the mixture was stirred with heating at 60° C. for 12 hr. The reaction mixture was concentrated under reduced pressure, and the residue was diluted with ethyl acetate (500 mL), and washed with water (200 mL) and saturated brine (200 mL). The organic layer was dried over anhydrous sodium sulfate, the insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. The obtained residue was recrystallized from ethyl acetate, hexane and diisopropyl ether to give the title compound (2.98 g, 83%) as a colorless powder.

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. additionthe residue was diluted with ethyl acetate (500 mL)
3. washwashed with water (200 mL) and saturated brine (200 mL)
4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
5. filtrationthe insoluble material was filtered off
6. concentrationthe filtrate was concentrated under reduced pressure
7. customThe obtained residue was recrystallized from ethyl acetate, hexane and diisopropyl ether