反应详情

温度

80 °C

A mixture of 3-amino-5-chloro-pyrazine-2-carboxylic acid methyl ester [28643-16-5] (2 g, 10.66 mmol), lithium chloride (1.582 g, 37.3 mmol), Pd(PPh3)2Cl2 (0.748 g, 1.066 mmol) and tributyl-((Z)-2-ethoxy-vinyl)-stannane (6.42 ml, 19.19 mmol) in DMF (104 ml) under argon was heated at 80° C. bath temperature for 1.5 h. A saturated. aq. NH4Cl was added and the mixture was extracted with MTBE, then once with EtOAc/THF 3/1. The combined organic layer was washed with brine, dried with Na2SO4, filtered and concentrated under reduced pressure. The residue was purified by chromatography on silica gel (cyclohexane to cyclohexane/EtOAc 1:9) to provide the title compound as yellow oil (1.96 g).

1. extractionthe mixture was extracted with MTBE
2. washThe combined organic layer was washed with brine
3. dry with materialdried with Na2SO4
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified by chromatography on silica gel (cyclohexane to cyclohexane/EtOAc 1:9)