HRID1436681

反应详情

EQUATION

反应方程式

HRID 1436681 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

Add THF (3 mL), N-methyl-N-propyl-5-tributylstannanyl-isophthalamic acid methyl ester (0.524 g, 1.00 mmol), nicotinoyl chloride hydrochloride (0.232 g, 1.30 mmol), 2-(di-tert-butylphosphino)biphenyl (0.045 g, 0.151 mmol), bis(dibenzylidene-acetone)palladium (0) (029 g, 0.05 mmol) to a sealed tube flushed with nitrogen. Heat the mixture at 50° C. for 16 h and cool to room temperature. Filter the mixture though a filtering agent, concentrate and purify (silica gel chromatography, eluting with 50:50 to 100:0 ethyl acetate:hexanes) to give the title compound (0.070 g, 21%).

WORKUP

后处理

  1. customflushed with nitrogen
  2. temperaturecool to room temperature
  3. filtrationFilter the mixture though a filtering agent
  4. concentrationconcentrate
  5. custompurify
  6. wash(silica gel chromatography, eluting with 50:50 to 100:0 ethyl acetate:hexanes)