METHYL 4-(3-NITRO-2-PYRIDINYL)BENZENECARBOXYLATE synthesis

Yield:937601-36-0 85%

Reaction Conditions:

with tetrakis(triphenylphosphine) palladium⁽⁰⁾;potassium carbonate in 1,4-dioxane;water at 90;Inert atmosphere;

Steps:

2.1 1) Synthesis of intermediate A2-2:

2-Chloro-3-nitropyridine (316 mg, 2 mmol),Methyl 4-borate benzoate (432 mg, 2.4 mmol),Pd(PPh3)4 (185 mg, 0.16 mmol) and potassium carbonate (552 mg, 4 mmol)Add to 1,4-dioxane (20mL) and water(4 mL) in a mixed solvent, nitrogen-protected, and reacted at 90 ° C overnight.Dilute with ethyl acetate (100 mL) and wash with brine (50 mL).The organic phase is dried over anhydrous sodium sulfate, filtered and concentrated.Purified by column chromatography(petroleum ether: ethyl acetate = 20:1 to 10:1),Get a yellow solid(440 mg, 85%).

References:

CN109553617,2019,A Location in patent:Paragraph 0080; 0081; 0082; 0083; 0084