反应详情

温度

140 °C

2-chloro-1,5-naphthyridine (10-1) (35 g, 213 mmol) in toluene (420 mL) was treated with tributyl(vinyl)stannane (101 g, 93.4 mL, 319 mmol) and tetrakis(triphenylphosphine)palladium (36.9 g, 31.9 mmol). The mixture was heated at 140° C. under microwave irradiation for 20 min, then cooled and concentrated in vacuo. The residue was purified by silica gel flash column chromatography, eluting with 0-100% EtOAc/heptane. The fractions containing the desired product (10-2) were pooled, and after solvent removal in vacuo, 19 g (57%) of the product were obtained. LC/MS: m/z (M+H)=157.2.

1. temperaturecooled
2. concentrationconcentrated in vacuo
3. customThe residue was purified by silica gel flash column chromatography
4. washeluting with 0-100% EtOAc/heptane
5. additionThe fractions containing the desired product (10-2)
6. customafter solvent removal in vacuo