3-chloro-2-methyl-5-nitro-pyridine synthesis

Yield:51984-62-4 344 mg

Reaction Conditions:

with tetrakis(triphenylphosphine) palladium⁽⁰⁾;caesium carbonate in 1,4-dioxane at 100; for 6 h;

Steps:

362.1 1st step

Cesium carbonate (338 mg), methylboronic acid (47 mg), and tetrakis(triphenylphosphine)palladium (60 mg) were added to a 1,4-dioxane (3 ml) solution containing 2,3-dichloro-5-nitropyridine (100 mg), followed by stirring at 100°C for 6 hours.
The reaction solution was adjusted to room temperature, and water was added, followed by extraction with ethyl acetate.
The resultant was washed with saturated saline and dried over anhydrous sodium sulfate, the solvent was distilled away under reduced pressure, and 3-chloro-2-methyl-5-nitropyridine (344 mg) was thus obtained.

References:

EP2589592,2018,B1 Location in patent:Paragraph 1190; 1191