反应详情

温度

90 °C

To a solution of 2,5-dichloropyridin-4-ol (CAN 847664-65-7, 1.5 g, 9.15 mmol) in DMF (15 ml) in a microwave vial were added cesium carbonate (4.47 g, 13.7 mmol) and 2,2,2-trifluoroethyl trifluoromethanesulfonate (3.18 g, 13.7 mmol). The vial was sealed and heated at 90° C. overnight. The reaction mixture was diluted with ethylacetate and extracted with water. The organic phase was collected and the aqueous phase was back-extracted with ethylacetate. Organic phases were combined, dried over magnesium sulfate and concentrated in vacuo. The residue was purified by flash chromatography eluting with a heptane/ethylacetate gradient on silica to yield the titled compound as a colorless oil (1.33 g, 59%). MS (ESI, m/z): 246.2 (M+H+).

1. customThe vial was sealed
2. extractionextracted with water
3. customThe organic phase was collected
4. extractionthe aqueous phase was back-extracted with ethylacetate
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated in vacuo
7. customThe residue was purified by flash chromatography
8. washeluting with a heptane/ethylacetate gradient on silica