反应详情

温度

80 °C

A mixture of ethyl ({[5-(3-{[(1,3-dimethyl-1H-pyrazol-5-yl)carbonyl]amino}-5-methylphenoxy)pyridin-2-yl]amino}carbonothioyl)carbamate (2.65 g, 4.76 mmol), hydroxylammonium chloride (2.96 g, 42.5 mmol), N,N-diisopropylethylamine (5.00 mL, 28.7 mmol), ethanol (100 mL) and methanol (100 mL) was stirred at 80° C. for 14 hr. The reaction solution was concentrated under reduced pressure. Ethyl acetate was added to the residue, and the mixture was washed with water and saturated brine, dried over anhydrous magnesium sulfate and filtrated. The filtrate was concentrated under reduced pressure and washed with ethanol-ethyl acetate to give the title compound (1.29 g, 72%) as a white solid.

1. concentrationThe reaction solution was concentrated under reduced pressure
2. additionEthyl acetate was added to the residue
3. washthe mixture was washed with water and saturated brine
4. dry with materialdried over anhydrous magnesium sulfate
5. filtrationfiltrated
6. concentrationThe filtrate was concentrated under reduced pressure
7. washwashed with ethanol-ethyl acetate