HRID1187056
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of 5-bromo-4-iodo-2-benzofuran-1(3H)-one (1 g, 2.95 mmol), potassium vinyltrifluoroborate (474 mg, 3.54 mmol) and Pd(dppf)Cl2 (200 mg) in 20 mL of TEA and 20 mL of EtOH was heated to reflux under N2 for 2 hours. TLC showed complete reaction. Most of the solvent was removed, and the residue was dissolved in EtOAc (100 mL). The solution was washed with 0.1 N HCl, sodium bicarbonate, and brine, dried over sodium sulfate, filtered and concentrated to provide 5-bromo-4-vinyl-2-benzofuran-1(3H)-one.
WORKUP
后处理
- temperaturewas heated
- temperatureto reflux under N2 for 2 hours
- customreaction
- customMost of the solvent was removed
- dissolutionthe residue was dissolved in EtOAc (100 mL)
- washThe solution was washed with 0.1 N HCl, sodium bicarbonate, and brine
- dry with materialdried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated