HRID747765

反应详情

EQUATION

反应方程式

HRID 747765 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

197 mg (0.26 mmol)) of 3-[(2S)-2-(benzenesulfonylamino)-3-[4-(1-benzyloxycarbonyl-4-piperidyloxy)phenyl]propoxy]-4-iodobenzonitrile and 74.4 mg (0.52 mmol) of methyl 2-acetaminoacrylate were dissolved in 6 ml of acetonitrile. 7.3 mg (0.03 mmol) of palladium (II) acetate, 55 mg (0.18 mmol) of tri-o-tolylphosphine and 96 mg (0.52 mmol) of tributylamine were added to the solution, and they were heated under reflux overnight. The solvent was distilled off and the residue was treated with ethyl acetate as the extractant in an ordinary manner to obtain the crude product, which was purified by the silica gel column chromatography to obtain the title compound.

WORKUP

后处理

  1. temperaturewere heated
  2. temperatureunder reflux overnight
  3. distillationThe solvent was distilled off
  4. additionthe residue was treated with ethyl acetate as the extractant in an ordinary manner
  5. customto obtain the crude product, which
  6. customwas purified by the silica gel column chromatography