HRID1848516

反应详情

EQUATION

反应方程式

HRID 1848516 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 5-bromo-4-cyclopropyl-2-benzofuran-1(3H)-one (760 mg, 3.004 mmol), potassium vinyltrifluoroborate (805 mg, 6.01 mmol) and Pd(dppf)Cl2 (100 mg) in 20 mL of TEA and 20 mL of EtOH was heated to reflux under N2 for 8 hours. After TLC showed complete reaction, then 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. The resulting oil was purified by column chromatography to give the title compound.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux under N2 for 8 hours
  3. customreaction
  4. custommost of the solvent was removed
  5. dissolutionthe residue was dissolved in EtOAc (100 mL)
  6. washThe solution was washed with 0.1 N HCl, sodium bicarbonate, and brine
  7. dry with materialdried over sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated
  10. customThe resulting oil was purified by column chromatography