反应详情

温度

60 °C

2-Chloro-6-methyl-4-methylthio-3-nitropyridine (2.80 g, 12.81 mmol) was dissolved in 2-methoxyethanol (40 mL). Potassium carbonate (1.90 g, 13.75 mmol) was added to the solution, followed by stirring for 5 hours at 60° C. The mixture was allowed to stand for cooling. Subsequently, the resultant mixture was extracted with ether-water, and the organic layer was washed with saturated brine, followed by drying sodium sulfate anhydrate and concentration under reduced pressure. The obtained residue was purified through silica gel column chromatography [(1) (eluent: n-hexane/ethyl acetate=4/1→n-hexane/ethyl acetate=2/1), (2) (eluent: chloroform)], to thereby yield 2-[(2-methoxyethyl)oxy]-6-methyl-4-methylthio-3-nitropyridine as a pale yellow oil (2.21 g, 67%).

1. temperaturefor cooling
2. extractionSubsequently, the resultant mixture was extracted with ether-water
3. washthe organic layer was washed with saturated brine
4. customby drying
5. concentrationsodium sulfate anhydrate and concentration under reduced pressure
6. customThe obtained residue was purified through silica gel column chromatography [(1) (eluent: n-hexane/ethyl acetate=4/1→n-hexane/ethyl acetate=2/1), (2) (eluent: chloroform)]