反应详情

温度

100 °C

To a 500 ml flask containing a stir bar was added 5-(2-hydroxyethyl)-6-iodo-2-benzofuran-1(3H)-one (5 g, 16.4 mmol), Potassium vinyltrifluoroborate (3.3 g, 24.7 mmol), Pd(dppf)Cl2 (0.6 g, 0.822 mmol) and TEA (2.3 mL). The mixture was then dissolved in EtOH (50 mL) and heated at 100° C. in a silicon oil bath for 2 h; TLC showed complete reaction. The flask was cooled to room temperature, treated with EtOAc (150 mL) and poured into a separatory funnel and washed with brine (2×100 mL). The organic layer was then separated, dried (Na2SO4), filtered and concentrated to dryness. The resulting organic residue was dissolved in DCM and absorbed into silica gel and purified by MPLC (hexanes/EtOAc; 1/1 eluent) to provide 5-(2-Hydroxyethyl)-6-vinyl-2-benzofuran-1(3H)-one.

1. additionTo a 500 ml flask containing a stir bar
2. customreaction
3. temperatureThe flask was cooled to room temperature
4. additionpoured into a separatory funnel
5. washwashed with brine (2×100 mL)
6. customThe organic layer was then separated
7. dry with materialdried (Na2SO4)
8. filtrationfiltered
9. concentrationconcentrated to dryness
10. dissolutionThe resulting organic residue was dissolved in DCM
11. customabsorbed into silica gel
12. custompurified by MPLC (hexanes/EtOAc; 1/1 eluent)