反应详情

温度

5 °C

NaH (52.6 mmol) was slowly added at 5° C. to a solution of 5-chloro-2-hydroxy-3-nitropyridine [21427-61-2] (43.8 mmol) and the mixture was stirred at 5° C. for 30 min. Methyl iodide (65.7 mmol) was added and the mixture was stirred at rt for 20 h. The mixture was diluted with H2O and extracted with EtOAc (3×). The combined organic phases were washed successively with H2O and brine, dried (Na2SO4), filtered and concentrated to afford the title compound. ESI-MS: tR=0.55 min, [M+H]+ 189/191 (LC-MS 1).

1. stirringthe mixture was stirred at rt for 20 h
2. extractionextracted with EtOAc (3×)
3. washThe combined organic phases were washed successively with H2O and brine
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated