تفاعل #45606

معادلة التفاعل

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

diisopropylethylamine

cyclopropanecarbonyl chloride

→

compound

المردود 97.3%

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

المردود 97.3%

المذيبات

ethyl acetate

ethyl acetate

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر