反应详情

温度

80 °C

The title compound was prepared from [2,3′]bipyridinyl-4-carboxylic acid methyl ester [prepared by the following procedure: A mixture of pyridine-3-boronic acid (0.7 g, 5.7 mmol), 2-bromo-isonicotinic acid (1.15 g, 5.7 mmol) and K2CO3 (0.63 g, 4.6 mmol) in CH3CN (120 mL)/H2O (10 mL) was degassed and Pd(PPh3)4 (0.13 g, 0.11 mmol) was added. The mixture was stirred for 24 h at 80° C. in an atmosphere of nitrogen and then concentrated in vacuum to a volume of about 10 ml. The pH was set to 6 by addition of 3N HCl and the solution was then evaporated in vacuum to dryness. The residue was stirred in 1N HCl-MeOH (23 ml) for 65 h at 50° C. The crude product was purified by chromatography (silica gel, AcOEt/cyclohexane 1:1) to give the methyl ester as light yellow oil (0.37 g).] (044 g, 2.1 mmol) by treatment with lithium tert-butyl acetate according to general procedure K (method b). Obtained as a light yellow oil (0.62 g, crude product).

1. customprepared by the following procedure
2. customwas degassed
3. concentrationconcentrated in vacuum to a volume of about 10 ml
4. additionThe pH was set to 6 by addition of 3N HCl
5. customthe solution was then evaporated in vacuum to dryness
6. stirringThe residue was stirred in 1N HCl-MeOH (23 ml) for 65 h at 50° C
7. customThe crude product was purified by chromatography (silica gel, AcOEt/cyclohexane 1:1)