反应详情

To a stirred suspension of 3-fluoro-2-hydroxy-5-nitropyridine (2.03 g, 12.84 mmol) and K2CO3 (3.55 g, 25.7 mmol) in DMF (20 mL) under Ar was added MeI (1.20 mL, 19.26 mmol). The reaction mixture was stirred for 1 hr at rt, concentrated, diluted with water (100 mL), and extracted with CH2Cl2. (2×150 mL) The combined organic layers were washed with water, dried over Na2SO4 and evaporated to afford the crude title product (2.06 g, 11.97 mmol, 93% yield) as a yellow solid. tR: 2.22 min (HPLC 1); tR: 0.49 min (LC-MS 2); ESI-MS: 173 [M+H]+ (LC-MS 2).

1. concentrationconcentrated
2. additiondiluted with water (100 mL)
3. extractionextracted with CH2Cl2
4. wash(2×150 mL) The combined organic layers were washed with water
5. dry with materialdried over Na2SO4
6. customevaporated