反应详情

温度

80 °C

Secondary amine 24 (200 mg, 0.41 mmol), DIPEA (110 μL, 0.62 mmol), and 2-chloro-pyrimidine (62 mg, 0.53 mmol) were dissolved in DMF (4 mL) and stirred at 80° C. After 12 h, the reaction mixture was cooled to ambient temperature, diluted with water, and extracted with EtOAc. The combined organic extracts were washed with brine and dried over anhydrous Na2SO4, filtered, and concentrated. The crude product was purified by flash silica gel chromatography (1:1 hexanes/EtOAc) to afford 140 mg (60%) of 29 as a colorless oil. Mass spectrum, m/z [566.0] (M+H)+.

1. temperaturethe reaction mixture was cooled to ambient temperature
2. extractionextracted with EtOAc
3. washThe combined organic extracts were washed with brine
4. dry with materialdried over anhydrous Na2SO4
5. filtrationfiltered
6. concentrationconcentrated
7. customThe crude product was purified by flash silica gel chromatography (1:1 hexanes/EtOAc)