Reaktion #45606

Reaktionsgleichung

2-Amino-5-bromo-4-fluoro-3-hydroxy-6-methylbenzonitrile

diisopropylethylamine

cyclopropanecarbonyl chloride

→

compound

Ausbeute 97.3%

2-Amino-5-bromo-3-cyano-6-fluoro-4-methylphenyl acetate

Ausbeute 97.3%

Lösungsmittel

ethyl acetate

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas added to the reaction liquid
2. 2
   Waschenby washing with water and saturated brine
3. 3
   EinengenThe organic layer was concentrated under reduced pressure
4. 4
   Sonstigethe resulting residue was recrystallized with diisopropyl ether/ethyl acetate

Vorschrift

2-Amino-5-bromo-4-fluoro-3-hydroxy-6-methylbenzonitrile (I-75) (7.86 g, 32.08 mmol) and diisopropylethylamine (19.5 ml, 112.2 mmol) were dissolved in ethyl acetate (300 ml), and at 0° C., cyclopropanecarbonyl chloride (4.4 ml, 48.12 mmol) was dropwise added, followed by stirring at room temperature for 16 hours under nitrogen atmosphere. After the reaction, ethyl acetate was added to the reaction liquid, followed by washing with water and saturated brine. The organic layer was concentrated under reduced pressure, the resulting residue was recrystallized with diisopropyl ether/ethyl acetate to obtain the entitled compound (8.96 g, 89%) as a white solid.

Quelle