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Sodium metal (0.119g, 5.1mmol) was dissolved in methanol (6ml) at 0°C (ice bath), <strong>[22280-60-0]6-chloro-2-methyl-3-nitro-pyridine</strong> (0.30g, 1.7mmol) was added and the mixture was stirred at 0°C until the complete consumption of <strong>[22280-60-0]6-chloro-2-methyl-3-nitro-pyridine</strong> (4h). Acetic acid (0.306g, 5.1mmol) was added and the solution was concentrated under reduced pressure. The residue was dissolved in ethyl acetate (20 ml), washed with water (10 ml), dried over anhydrous Na2SO4, filtered and the solvent was removed under reduced pressure to give 0.28g (97percent) 6-methoxy-2-methyl-3-nitropyridine as colourless powder.
With sodium; In methanol; (2S)-N-methyl-1-phenylpropan-2-amine hydrate;
6-methoxy-3-nitro-2-picoline 0.46 gm (20 mMol) sodium were dissolved in 15 mL anhydrous methanol. To this solution were added 2.3 gm 6-chloro-3-nitro-2-picoline in portions. The resulting mixture was stirred for 18 hours at room temperature and then 1 hour at reflux. The reaction mixture was poured into 100 mL of ice water with vigorous stirring. The suspension was filtered and the solid dried at 30° C. under reduced pressure for 18 hours to provide 2.04 gm (91percent) of the desired compound as a tan solid.
2.04 gm (91%)
With sodium; In methanol; (2S)-N-methyl-1-phenylpropan-2-amine hydrate;
6-methoxy-3-nitro-2-picoline 0.46 gm (20 mMol) sodium were dissolved in 15 mL anhydrous methanol. To this solution were added 2.3 gm 6-chloro-3-nitro-2-picoline in portions. The resulting mixture was stirred for 18 hours at room temperature and then 1 hour at reflux. The reaction mixture was poured into 100 mL of ice water with vigorous stirring. The suspension was filtered and the solid dried at 30°C under reduced pressure for 18 hours to provide 2.04 gm (91percent) of the desired compound as a tan solid.
In methanol;
Preparation 6 2-Methoxy-5-Nitro-6-Methylpyridine Sodium metal (8.68 g, 378 mmol) was added to methanol (350 mL) pre-cooled to 0° C. After the sodium completely dissolved, <strong>[22280-60-0]2-chloro-5-nitro-6-methylpyridine</strong> (40.78 g, 236 mmol) was slowly added as a solid. The reaction mixture was heated at reflux temperature overnight, then poured into ice-water. The product was filtered and dried in vacuo overnight to give 29.39 grams of the title compound. (73percent).
Step 3 6-Methoxy-2-memyl~3-mtropyridineA roundbottom flask was charged with a solution of 6-chloro-2-methyl-3- nitropyridine (12.0 g, 69.36 mmol) in methanol (100 ml). Sodium methanolate (5.6 g, 103.70 mmol) was added and the resulting solution was stirred at room temperature for 24 hours. The mixture was poured into 100 ml of water and the solids that formed were collected by filtration to afford the title compound.
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