2-(4-CHLOROPHENYL)-3-NITROPYRIDINE synthesis

Yield:886361-74-6 97.4%

Reaction Conditions:

with tetrakis(triphenylphosphine) palladium⁽⁰⁾;potassium carbonate in 1,4-dioxane;water;Inert atmosphere;Reflux;

Steps:

3.1 Step 1: Synthesis of Intermediate K

Under the protection of nitrogen, the intermediate J (12.0g, 75.69mmol), 4-chloro-phenylboronic acid (14.2g, 90.83mmol), Pd(PPh₃)₄(2.62g2.27mmol)K₂CO₃(20.92g,151.38mmol)Dioxane(240mL)H₂O (60 mL) was placed in a three-necked flask and heated to reflux overnight.After the reaction is complete, cool to room temperature, add distilled water, extract the mixture with DCM, wash the organic phase with water, dry the organic phase with anhydrous magnesium sulfate, spin off the solvent under reduced pressure, and purify by silica gel column chromatography (eluent: PE/DCM=1: 1), the bright yellow solid intermediate K (17.3 g, 73.73 mmol) was obtained, and the yield was 97.4%.

References:

CN111675707,2020,A Location in patent:Paragraph 0142-0145