反应详情

To a two-layer solution of 5-amino-2-chloro-4-fluorophenol (3.50 g, 21.7 mmol) in tetrahydrofuran (35 mL)/1N aqueous sodium hydrogen carbonate solution (65 mL) was added a solution of 3-(1-cyano-1-methylethyl)benzoyl chloride synthesized above in tetrahydrofuran (30 mL), and the mixture was stirred at room temperature for 4 hr. The aqueous layer was separated, and extracted with ethyl acetate (200 mL). The combined organic layer was washed with water (100 mL) and saturated brine (100 mL), and dried over anhydrous sodium sulfate. The insoluble material was filtered off, and the filtrate was concentrated under reduced pressure to give the title compound (5.18 g, 72%) as a gray powder.

1. customThe aqueous layer was separated
2. extractionextracted with ethyl acetate (200 mL)
3. washThe combined organic layer was washed with water (100 mL) and saturated brine (100 mL)
4. dry with materialdried over anhydrous sodium sulfate
5. filtrationThe insoluble material was filtered off
6. concentrationthe filtrate was concentrated under reduced pressure