反応 #45606

反応方程式

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

diisopropylethylamine

cyclopropanecarbonyl chloride

→

compound

収率 97.3%

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

収率 97.3%

溶媒

ethyl acetate

ethyl acetate

反応条件

後処理

1. 1
   workup.ADDITIONwas added to the reaction liquid
2. 2
   洗浄by washing with water and saturated brine
3. 3
   濃縮The organic layer was concentrated under reduced pressure
4. 4
   その他the resulting residue was recrystallized with diisopropyl ether/ethyl acetate

実験手順

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.

出典