2,5-Dimethyl-3-nitropyridine synthesis
- Product Name:2,5-Dimethyl-3-nitropyridine
- CAS Number:52381-06-3
- Molecular formula:C7H8N2O2
- Molecular Weight:152.15
Yield:52381-06-3 78%
Reaction Conditions:
with potassium carbonate;tetrakis(triphenylphosphine) palladium(0) in 1,4-dioxane; for 7.5 h;Inert atmosphere;Reflux;
Steps:
2.2
(2); Tetrakis(triphenylphosphine)Palladium(0) (0.57 mmol, 656 mg), potassium carbonate (34.06 mmol, 4.71 g) and trimethylboroxine (17.03 mmol, 4.275 g) were successively added to a dioxane solution (15 ml) of 2,5-dibromo-3-nitropyridine (5.68 mmol, 1.6 g) in argon atmosphere, followed by stirring under heat refluxing for 7.5 hours. Water was added to the resulting reaction mixture on ice, followed by extracting with ethyl acetate. An organic layer was washed with saturated saline, dried over anhydrous sodium sulfate, and filtered, followed by distilling away a solvent under reduced pressure. The resulting crude product was purified with column chromatography to obtain 671 mg of 2,5-dimethyl-3-nitropyridine (yield 78%). 1H NMR δ ppm (300 MHz, CDCl3) data of this compound are 8.53 (s, IH), 8.07 (s, IH), 2.80 (s, 3H), 2.41 (s, 3H).
References:
WO2009/88103,2009,A1 Location in patent:Page/Page column 17
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