反应详情

温度

5 °C

A mixture of NaH (577 mg, 14.4 mmol) and 5-chloro-2-hydroxy-3-nitropyridine (2.1 g, 12.0 mmol) in DMF (21 mL) was stirred for 1 h at 5° C. Methyl iodide (1.1 mL, 18.0 mmol) was added. The resulting mixture was allowed to warm to rt, stirred overnight, cooled to 0° C., quenched by addition of water, and extracted with EtOAc. The organic layer was dried (Na2SO4), filtered, and concentrated. The residue was used without further purification. tR: 0.61 min (LC-MS 2); ESI-MS: 189.1/191.1 [M+H]+ (LC-MS 2).

1. temperatureto warm to rt
2. stirringstirred overnight
3. temperaturecooled to 0° C.
4. customquenched by addition of water
5. extractionextracted with EtOAc
6. dry with materialThe organic layer was dried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated
9. customThe residue was used without further purification