反应详情

温度

80 °C

A mixture of ethyl [(5-methoxypyridin-2-yl)carbamothioyl]carbamate (1.34 g, 5.25 mmol), hydroxylammonium chloride (2.55 g, 36.7 mmol), N,N-diisopropylethylamine (4.57 mL, 26.2 mmol), ethanol (15 mL) and methanol (15 mL) was stirred at 80° C. for 8 hr. The reaction mixture was diluted with water, and extracted with ethyl acetate (×3). The combined organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and filtered. The filtrate was concentrated under reduced pressure, and the residue was collected by filtration, and washed with ethyl acetate-hexane to give the title compound (790 mg, 92%) as a yellow oil.

1. extractionextracted with ethyl acetate (×3)
2. washThe combined organic layer was washed with saturated brine
3. dry with materialdried over anhydrous magnesium sulfate
4. filtrationfiltered
5. concentrationThe filtrate was concentrated under reduced pressure
6. filtrationthe residue was collected by filtration
7. washwashed with ethyl acetate-hexane