反应详情

Potassium tert-butoxide (236 mg, 2.106 mmol, 1.5 eq), compound 354a) (500 mg, 1.404 mmol, 1.0 eq) and 2-chloro-5-(2-fluorophenyl)pyrimidine (292 mg, 1.404 mmol, 1.0 eq) in DMF (10 mL) were stirred at 120° C. for 5 h. The reaction mixture was cooled to room temperature, diluted with water (15 mL), and extracted with ethyl acetate (2×20 mL). The combined organic layers were washed with brine (30 mL), dried over sodium sulfate and concentrated. The residue was purified by silica gel column chromatography [100-200 mesh silica; ethyl acetate/pet ether=7:3]. Yield: 400 mg (53% of theory).

1. extractionextracted with ethyl acetate (2×20 mL)
2. washThe combined organic layers were washed with brine (30 mL)
3. dry with materialdried over sodium sulfate
4. concentrationconcentrated
5. customThe residue was purified by silica gel column chromatography [100-200 mesh silica; ethyl acetate/pet ether=7:3]