Reaktion #45575

Reaktionsgleichung

potassium carbonate

N-(2-bromo-5-cyano-3-methoxy-6-methylbiphenyl-4-yl)2,2,2-trifluoroacetamide

→

compound

Ausbeute 94.0%

4-Amino-6-bromo-5-methoxy-2-methylbiphenyl-3-carbonitrile

Ausbeute 94.0%

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturAfter cooling
2. 2
   Sonstigemethanol was evaporated away under reduced pressure
3. 3
   Extraktionfollowed by extraction with ethyl acetate
4. 4
   Waschenwashing with saturated brine
5. 5
   Trocknendrying on anhydrous magnesium sulfate
6. 6
   Einengenthe solvent was concentrated under reduced pressure
7. 7
   Sonstigeto obtain a pale brown residue
8. 8
   SonstigeThe resulting residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=6:1)

Vorschrift

Aqueous potassium carbonate solution (1.25 ml) [potassium carbonate (15 g) was dissolved in water (100 ml)] and methanol (1.25 ml) were added to N-(2-bromo-5-cyano-3-methoxy-6-methylbiphenyl-4-yl)2,2,2-trifluoroacetamide (I-38) (133 mg, 0.322 mmol), followed by stirring overnight at 70° C. After cooling, methanol was evaporated away under reduced pressure, followed by extraction with ethyl acetate, washing with saturated brine and drying on anhydrous magnesium sulfate, the solvent was concentrated under reduced pressure to obtain a pale brown residue. The resulting residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=6:1) to obtain the entitled compound (95 mg, 94%) as a colorless solid.

Quelle