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With silver(I) acetate; palladium diacetate; Trimethylacetic acid; at 140℃; for 18h;Inert atmosphere;
Under a nitrogen atmosphere, palladium acetate (11.2 mg, 0.05mmol), 1, 10 - phenanthroline (49.6 mg, 0.25mmol), silver acetate (250 mg, 1.5mmol), (1 ml) was suspended in pyridine (51.1 mg, 0.5mmol) pivalic acid, stirred at 140 °C 26 hours. After the reaction mixture was cooled to room temperature, the insoluble matter was removed by filtration over celite, methylene chloride (10 ml) was washed. The filtrate was concentrated under reduced pressure, 1, 1, 2, 2 - tetrachloroethane (15.8 mul, 0.15mmol) was added as an internal standard substance was obtained residue,1H NMR (88percent) yield was calculated based oxidizing agent. (Methylene chloride/hexane=5/95) to give a residue for a thin layer chromatography analysis, the subject compound (quantitative value NMR 89percent, 80percent isolated yield) was obtained as a white powder 93.1 mg.
To cone. H2SO4 (5 mL) chilled in an ice bathm is added 4-methoxypyridine (0.5 mL, 4.9 mmol) dropwise over a 20 s period. Cone. Fuming nitric acid (5 mL) is added, and the reaction mixture is heated at 70 °C for 2.5 days. This mixture is cooled to rt, and then is poured into ice. Soild K2CO3 is added until the pH of the mixture is basic. The mixture is partitioned between H20 and EtOAc. The two layers is separated, and the aqueous layer is extracted with EtOAc once. The combined organic layers are washed with H2O and brine, dried over MgS04, filtered, and concentrated in vacuo to yield 0.7 g (92percent) of the product a yellow powder. 1H NMR (CDC13, 300 MHz) delta 9.02 (s, 1H), 8.65 (d, J= 5.8, 1 H), 7.04 (d, J = 5.9, 1H), 4.05 (s, 3H). LC Rt: 0.5 min; LCMS m/z 155 (M+l, 100percent).
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