反应详情

5-methyl-3-nitro-pyridin-2-ol (5 g, 32.4 mmol) and benzyltrimethyl ammonium chloride (3.01 g, 16.2 mmol) were dissolved in acetonitrile, and phosphorus oxychloride (9.0 ml, 97.2 mmol) was added thereto and stirred at 800 for 6 hours. The reaction mixture was cooled and poured into ice water to quench the reaction, and extracted with dichloromethane. The combined organic layer was washed with saturated saline solution, dried over anhydrous sodium sulfate (Na2SO4), filtered and evaporated under reduced pressure. The residue was purified by column chromatography on silica eluting with a solvent of dichloromethane. The fractions containing the product were collected and evaporated to obtain 2-chloro-5-methyl-3-nitro-pyridine as yellow solid (5.39 g, 97%).

1. temperatureThe reaction mixture was cooled
2. customto quench
3. customthe reaction
4. extractionextracted with dichloromethane
5. washThe combined organic layer was washed with saturated saline solution
6. dry with materialdried over anhydrous sodium sulfate (Na2SO4)
7. filtrationfiltered
8. customevaporated under reduced pressure
9. customThe residue was purified by column chromatography on silica eluting with a solvent of dichloromethane
10. additionThe fractions containing the product
11. customwere collected
12. customevaporated