HRID1466833

反应详情

EQUATION

反应方程式

HRID 1466833 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Triisopropylsilanethiol (6.7 mL, 31.2 mmol) was dissolved in THF (75 mL) at 0° C. and sodium hydride (1.25 g, 60% dispersion in mineral oil, 31.3 mmol) was added, then the solution was allowed to warm to room temperature. Meanwhile, (3-bromo-4-methoxy-phenyl)-acetic acid ethyl ester (6.38 g, 23.4 mmol) was dissolved in THF (75 mL) and sparged with N2 (g). The first solution was added to the second and tetrakis(triphenylphosphine)palladium(0) (1.3 g, 1.1 mmol) was also added. The reaction was heated to reflux overnight then treated to standard aqueous workup. The residue was purified by silica gel chromatography (0-10% EtOAc in hexanes) to give the title compound.

WORKUP

后处理

  1. customsparged with N2 (g)
  2. additionwas also added
  3. temperatureThe reaction was heated
  4. temperatureto reflux overnight
  5. additionthen treated to standard aqueous workup
  6. customThe residue was purified by silica gel chromatography (0-10% EtOAc in hexanes)