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
To a 300 ml reaction vessel with a stirrer were fed 15 g of α-(3-(1-phenylethenyl)phenyl)propionic acid obtained in Example 2, 0.03 g of cobalt naphthenate and 100 ml of acetic acid as a solvent and 150 ml/min of pure oxygen was fed into the vessel for 16 hours at a reaction temperature of 120° C. After the reaction, the solvent was removed by reduced-pressure distillation to obtain a solid substance. The solid substance was washed five times with 500 ml of water and it was dissolved in 500 ml of ether and washed three times again with water. After that, the ether was removed by reduced-pressure distillation and the product was finally recrystallized with benzene/petroleum ether mixture to obtain 9.8 g of α-(3-benzoylphenyl)propionic acid (ketoprofen). The properties such as melting point and the spectrum of the final product were the same as those of an authentic sample.
WORKUP
后处理
- customTo a 300 ml reaction vessel with a stirrer
- customAfter the reaction
- customthe solvent was removed by reduced-pressure distillation
- customto obtain a solid substance
- washThe solid substance was washed five times with 500 ml of water and it
- dissolutionwas dissolved in 500 ml of ether
- washwashed three times again with water
- customAfter that, the ether was removed by reduced-pressure distillation
- customthe product was finally recrystallized with benzene/petroleum ether mixture