反应详情

温度

140 °C

2-Bromo-4-methylpyridine (400 mg, 2.326 mmol), tert-butyl 1,4-diazepane-1-carboxylate (2.1 g, 10.5 mmol) and potassium carbonate (2.8 g, 20 mmol) were combined in anhydrous DMF (20 ml) and heated under microwave heating at 140° C. for 5 hours. The mixture was poured into water and extracted with ethyl acetate (4×). The combined organic layers were washed with brine (2×) and dried over sodium sulfate. The solvent was removed under reduced pressure and the residue was purified two times by column chromatography (silica, gradient from 0 to 50% ethyl acetate in heptane) to yield 97 mg (0.33 mmol, 14%). MS (ESI) m/z=292.2 [M+1]+.

1. temperatureheated under microwave
2. extractionextracted with ethyl acetate (4×)
3. washThe combined organic layers were washed with brine (2×)
4. dry with materialdried over sodium sulfate
5. customThe solvent was removed under reduced pressure
6. customthe residue was purified two times by column chromatography (silica, gradient from 0 to 50% ethyl acetate in heptane)
7. customto yield 97 mg (0.33 mmol, 14%)