反应详情

To a solution of 3-chloro-2-hydroxy-5-nitropyridine [22353-38-4] (143 mmol) and K2CO3 (286 mmol) in DMF (250 mL) was added methyl iodide (215 mmol) at 0° C. and the reaction mixture was stirred at rt for 3 h. The reaction mixture was concentrated, diluted with H2O and extracted with EtOAc (2×). The combined organic layers were washed with H2O, dried (Na2SO4) and concentrated to afford the title compound as a yellow solid. tR: 2.90 min (HPLC 3); ESI-MS: tR=0.63 min, [M+H]+189/191 (LC-MS 1).

1. concentrationThe reaction mixture was concentrated
2. additiondiluted with H2O
3. extractionextracted with EtOAc (2×)
4. washThe combined organic layers were washed with H2O
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated