Water → N-{3-[(6-{[(4-methylphenyl)sulfonyl]amino}pyridin-3-yl)oxy]phenyl}-3-(trifluoromethyl)benzamide

Temperatur

80 °C

To a solution of N-{3-[(6-aminopyridin-3-yl)oxy]phenyl}-3-(trifluoromethyl)benzamide (2.00 g, 5.36 mmol) in pyridine (60 mL) was added 4-methylbenzenesulfonyl chloride (1.12 g, 5.89 mmol) under ice-cooling, and the mixture was stirred with heating at 80° C. for 2 days. After cooling the reaction mixture to room temperature, water (200 mL) was added, and the mixture was extracted with ethyl acetate (300 mL). The organic layer was washed with saturated brine (300 mL), and dried over anhydrous sodium sulfate. The insoluble material was filtered off, and the filtrate was concentrated under reduced pressure to give the title compound (2.75 g, 99%) as a yellow oil. The obtained compound was used for the next reaction without further purification.

1. temperaturecooling
2. temperatureAfter cooling the reaction mixture to room temperature
3. extractionthe mixture was extracted with ethyl acetate (300 mL)
4. washThe organic layer was washed with saturated brine (300 mL)
5. dry with materialdried over anhydrous sodium sulfate
6. filtrationThe insoluble material was filtered off
7. concentrationthe filtrate was concentrated under reduced pressure

ORD-Eintrag

ord-270dcd025627409a93adb462219142c1

Quelldatensatz

uspto-grants-2013_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08344135B2