HRID1931782
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe resulting mixture was heated under a reduced pressure of 8 kPa
- temperatureThe reaction mixture was heated for 5 hours
- customproduced
- customwas removed out of the reaction system
- temperatureAfter cooling
- customthe solvent was removed by distillation
- customa rotary evaporator
- distillationThe residue was then distilled under reduced pressure