反应详情

温度

100 °C

A mixture of 2-chloro-5-(methoxymethyl)pyridine (0.831 g, 5.27 mmol), tetrakis (1.219 g, 1.055 mmol), dicyanozinc (0.929 g, 7.91 mmol) and DMF (17.58 ml) was stirred at 100° C. for 3 hrs. The reaction was treated with water and extracted with EtOAc. The organic portion was dried over Na2SO4, filtered, and concentrated in vacuo. The crude material was purified by column chromatography, eluting with 10-40% EtOAc/Heptanes to give the title compound (550 mg, 3.71 mmol, 70.4%). MS m/z=149.1 (M+H).

1. extractionextracted with EtOAc
2. dry with materialThe organic portion was dried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customThe crude material was purified by column chromatography
6. washeluting with 10-40% EtOAc/Heptanes