反应详情

温度

60 °C

To a solution of hydroxylamine hydrochloride (400 mg, 5.76 mmol) and N,N-diisopropylethylamine (1.20 mL, 6.88 mmol) in methanol (8.0 mL)/ethanol (8.0 mL) was added ethyl ({[5-(3-{[3-(trifluoromethyl)benzoyl]amino}phenoxy)pyridin-2-yl]amino}carbonothioyl)carbamate (480 mg, 0.95 mmol) obtained above, 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 (100 mL). The mixture was washed with water (50 mL) and saturated brine (50 mL), and dried over anhydrous sodium sulfate. The insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate=50/50→0/100), and fractions containing the desired product were concentrated under reduced pressure to give the title compound (0.48 g, quantitative) as a pale-yellow powder.

1. customobtained above, and the mixture
2. concentrationThe reaction mixture was concentrated under reduced pressure
3. additionthe residue was diluted with ethyl acetate (100 mL)
4. washThe mixture was washed with water (50 mL) and saturated brine (50 mL)
5. dry with materialdried over anhydrous sodium sulfate
6. filtrationThe insoluble material was filtered off
7. concentrationthe filtrate was concentrated under reduced pressure
8. customThe obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate=50/50→0/100), and fractions
9. additioncontaining the desired product
10. concentrationwere concentrated under reduced pressure