Реакция #45606

Уравнение реакции

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

diisopropylethylamine

cyclopropanecarbonyl chloride

→

compound

Выход 97.3%

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

Выход 97.3%

Растворители

ethyl acetate

ethyl acetate

Условия реакции

Обработка

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

Методика

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.

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