Potassium Carbonate → HCID 67312595, Verbindung

Temperatur

80 °C

To a solution of 1,2-difluoro-4-nitrobenzene (1.19 g, 7.49 mmol) and 3-(1-cyano-1-methylethyl)-N-(5-hydroxy-2-methylphenyl)benzamide (2.0 g, 7.13 mmol) in N,N-dimethylformamide (15 mL) was added potassium carbonate (1.47 g, 10.7 mmol), and the mixture was stirred at 80° C. for 18 hr. The reaction mixture was cooled to room temperature, and concentrated under reduced pressure. The obtained residue was diluted with ethyl acetate (200 mL), washed with water (200 mL) and saturated brine (200 mL), successively, 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=95/5→0/30), and the obtained solution was concentrated under reduced pressure to give the title compound (2.09 g, 70%) as a yellow oil.

1. temperatureThe reaction mixture was cooled to room temperature
2. concentrationconcentrated under reduced pressure
3. additionThe obtained residue was diluted with ethyl acetate (200 mL)
4. washwashed with water (200 mL) and saturated brine (200 mL)
5. dry with materialsuccessively, and dried 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=95/5→0/30)
9. concentrationthe obtained solution was concentrated under reduced pressure

ORD-Eintrag

ord-dd197970bb9a46768ba55ff126ddd73b

Quelldatensatz

uspto-grants-2012_12

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08324395B2