反应详情

To a suspension of 10 g (63.6 mmol) 2-hydroxy-5-methyl-3-nitropyridine and 17.58 g (127 mmol) K2CO3 in 100 ml DMF, 5.96 ml (95 mmol) MeI was added at 0° C. Afterwards the reaction mixture was stirred at room temperature for 2 hours. The reaction mixture was concentrated, diluted with water and extracted three times with CH2Cl2. The organic layers were combined, dried over Na2SO4, filtered and concentrated to obtain an orange slurry. The residue was treated with ether and the precipitate was filtered off and dried under high vacuum to obtain 9.74 g (57.9 mmol, 91% yield) of the title compound as an orange solid. LCMS: (M+H)=169; tR=0.47 min (LC-MS 6). HPLC: tR=1.70 min (HPLC 8). 1H-NMR (DMSO-d6, 400 MHz) δ ppm 8.30 (d, 1H) 8.08 (m, 1H) 3.50 (s, 3H) 2.09 (s, 3H).

1. additionwas added at 0° C
2. concentrationThe reaction mixture was concentrated
3. additiondiluted with water
4. extractionextracted three times with CH2Cl2
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated
8. customto obtain an orange slurry
9. filtrationthe precipitate was filtered off
10. customdried under high vacuum