反应详情

温度

150 °C

2,6-Dichloro-4-methylpyridine (2.00 g, 12.3 mmol) was suspended in NMP (10 mL). N,N-Diisopropylethylamine (4.31 mL, 24.7 mmol) and benzylamine (1.42 mL, 13.0 mmol) were added, and the reaction mixture was heated to 150° C. in a microwave for 90 minutes. The reaction mixture was allowed to cool to room temperature, diluted with water, and extracted with diethyl ether (2×). The combined organics were dried over sodium sulfate, filtered, and concentrated under reduced pressure. The residue was purified via silica gel column chromatography (0-10% ethyl acetate/hexanes, linear gradient) to give N-benzyl-6-chloro-4-methylpyridin-2-amine. MS ESI calc'd. for C13H14ClN2 [M+H]+ 233. found 233.

1. temperatureto cool to room temperature
2. extractionextracted with diethyl ether (2×)
3. dry with materialThe combined organics were dried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified via silica gel column chromatography (0-10% ethyl acetate/hexanes, linear gradient)