反应详情

A suspension of tert-butyl{2-fluoro-5-[(5-nitropyridin-2-yl)oxy]phenyl}carbamate (3.49 g, 10 mmol) and 10% palladium-carbon (1.0 g) in methanol (20 mL)-tetrahydrofuran (20 mL) was vigorously stirred at room temperature under a hydrogen atmosphere overnight. The insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. The residue was poured into water (200 mL), and the mixture was extracted with ethyl acetate (100 mL×2). The ethyl acetate layers were combined, and dried over anhydrous sodium sulfate. The insoluble material was filtered off, and the filtrate was concentrated under reduced pressure, and the residue was triturated with diethyl ether to give the title compound (3.00 g, 94%) as a white amorphous.

1. filtrationThe insoluble material was filtered off
2. concentrationthe filtrate was concentrated under reduced pressure
3. additionThe residue was poured into water (200 mL)
4. extractionthe mixture was extracted with ethyl acetate (100 mL×2)
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 residue was triturated with diethyl ether