反应详情

A mixture of the 2-methyl-4-chloropyridine (1.00 g, 7.84 mmol), NBS (1.42 g, 8.00 mmol) and benzoyl peroxide (˜10 mg) in 10 mL of CCl4 was heated at reflux for 5 h. After cooling down, the reaction mixture was filtered and filtrate was concentrated to give the crude products mixture, which was dissolved in DMF and treated with morpholine (1.00 mL) and K2CO3 (1 g). The mixture was stirred overnight. The mixture was then diluted with EtOAc, washed with water, brine, dried over Na2SO4, filtered and concentrated in vacuo. The crude product was purified by column chromatography on SiO2 to give 400 mg of the desired 2-morpholinomethyl-4-chloropyridine.

1. temperaturewas heated
2. temperatureat reflux for 5 h
3. temperatureAfter cooling down
4. filtrationthe reaction mixture was filtered
5. concentrationfiltrate was concentrated
6. customto give the crude products mixture, which
7. washwashed with water, brine
8. dry with materialdried over Na2SO4
9. filtrationfiltered
10. concentrationconcentrated in vacuo
11. customThe crude product was purified by column chromatography on SiO2