Potassium Carbonate → Tert-butyl{4-chloro-2-fluoro-5-[(5-nitropyridin-2-yl)oxy]phenyl}carbamate

A mixture of tert-butyl(4-chloro-2-fluoro-5-hydroxyphenyl)carbamate (6.70 g, 25.6 mmol), 2-chloro-5-nitropyridine (4.06 g, 25.6 mmol), potassium carbonate (3.89 g, 28.1 mmol) and N,N-dimethylformamide (70 mL) was stirred at room temperature for 30 min. To the reaction mixture was added aqueous ammonium chloride solution (100 mL), and the mixture was extracted with ethyl acetate (150 mL×3). The organic layers were combined, and washed successively with water (100 mL) and saturated brine (50 mL), and dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to give the title compound (4.52 g, 46%) as a white powder.

1. extractionthe mixture was extracted with ethyl acetate (150 mL×3)
2. washwashed successively with water (100 mL) and saturated brine (50 mL)
3. dry with materialdried over anhydrous magnesium sulfate
4. concentrationconcentrated under reduced pressure

ORD-Eintrag

ord-278eacbf2fb342f9af72634729404735

Quelldatensatz

uspto-grants-2013_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08344135B2