反应详情

温度

90 °C

2-Chloro-5-cyanopyridine (477 mg, 3.4 mmol), tert-butyl (2-aminopropyl)carbamate (300 mg, 1.7 mmol) and potassium bicarbonate (345 mg, 3.4 mmol) are dissolved in DMF (10 ml) and stirred at 90° C. under argon for 12 h. The reaction mixture is diluted with water (100 ml) and extracted with ethyl acetate (3×75 ml). The combined organic phases are washed with saturated aqueous sodium chloride solution, dried over magnesium sulphate and concentrated. After removal of the solvent, the residue is purified by flash chromatography on silica gel (eluent: cyclohexane/ethyl acetate 10:1). 265 mg (55% of theory) of the product are obtained as a solid.

1. extractionextracted with ethyl acetate (3×75 ml)
2. washThe combined organic phases are washed with saturated aqueous sodium chloride solution
3. dry with materialdried over magnesium sulphate
4. concentrationconcentrated
5. customAfter removal of the solvent
6. customthe residue is purified by flash chromatography on silica gel (eluent: cyclohexane/ethyl acetate 10:1)
7. custom265 mg (55% of theory) of the product are obtained as a solid