HRID1777562

反应详情

EQUATION

反应方程式

HRID 1777562 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

1-(4-Amino-3-iodophenyl)ethanone (0.100 g; 0.383 mmol), 4-(3-fluorobenzyl)-N-(4-(triethylsilyl)but-3-ynyl)benzamide 0.151 g; 0.383 mmol), bis(diphenylphosphino)ferrocene]palladium(II) chloride (0.016 g; 0.019 mmol), lithium chloride (0.016 mg; 0.383 mmol) and sodium carbonate (0.081 g; 0.766 mmol) were suspended in DMF (5 mL) and the mixture was stirred at 100° C. for 18 hours. The solution was concentrated under reduced pressure and diluted in ethyl acetate. The organic layer was successively washed with brine, sodium thiosulfate, dried and concentrated under reduced pressure. The crude residue was purified by flash chromatography on silica gel (eluent 2 to 60% ethyl acetate in heptane) to afford 0.043 g (21%) of the title compound as a yellow oil.

WORKUP

后处理

  1. concentrationThe solution was concentrated under reduced pressure
  2. additiondiluted in ethyl acetate
  3. washThe organic layer was successively washed with brine, sodium thiosulfate
  4. customdried
  5. concentrationconcentrated under reduced pressure
  6. customThe crude residue was purified by flash chromatography on silica gel (eluent 2 to 60% ethyl acetate in heptane)