Reaktion #54316

Reaktionsgleichung

4-hydroxyphenylpropionic acid

potassium carbonate

4-hydroxyphenylpropionic acid

monochloroacetone

→

acetonyl 4-hydroxyphenylpropionate

Ausbeute 97.0%

Lösungsmittel

dichloroethane

dimethylformamide

dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.DISTILLATIONwas distilled off from the reaction solution
2. 2
   Sonstigeto give a residue
3. 3
   Waschenthe solution was washed with water
4. 4
   SonstigeThe layer of dichloroethane was removed
5. 5
   workup.DISTILLATIONthe solvent was distilled off

Vorschrift

After 49.9 g of 4-hydroxyphenylpropionic acid was dissolved in 160 ml of dimethylformamide, 21.8 g of potassium carbonate was added to the solution at room temperature. Then 29.1 g of monochloroacetone was added dropwise to the solution at 60° C. and the reaction with 4-hydroxyphenylpropionic acid was carried out at 80°-90° C. for 1 hour. After the reaction, dimethylformamide was distilled off from the reaction solution to give a residue. After the residue was dissolved in dichloroethane, the solution was washed with water. The layer of dichloroethane was removed and the solvent was distilled off to give 64.7 g (yield 97%) of acetonyl 4-hydroxyphenylpropionate. After recrystallization from isopropylether, the product was a colorless crystalline material having a melting point of 64.5° C.

Quelle