HRID1819730

反应详情

EQUATION

反应方程式

HRID 1819730 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In a 500-ml flask, 4-trifluoromethylaniline (80.6 g, 0.5 mol), methyl 3-oxopentanoate (65.1 g, 0.5 mol) and toluene 400 ml were placed. To this solution was added boron trifluoride etherate (1.42 g, 10 mmol), and the resulting mixture was heated under a reduced pressure of 8 kPa. The reaction mixture was heated for 5 hours under reflux, while water produced was removed out of the reaction system by using a Dean-Stark trap. Then, the heating was discontinued and nitrogen was leaked. After cooling, the solvent was removed by distillation by using a rotary evaporator. The residue was then distilled under reduced pressure to give 105.3 g of the title compound. The yield was 77.1%.

WORKUP

后处理

  1. temperaturethe resulting mixture was heated under a reduced pressure of 8 kPa
  2. temperatureThe reaction mixture was heated for 5 hours
  3. customproduced
  4. customwas removed out of the reaction system
  5. temperatureAfter cooling
  6. customthe solvent was removed by distillation
  7. customa rotary evaporator
  8. distillationThe residue was then distilled under reduced pressure