Reaktion #548585

Reaktionsgleichung

safrole

m-chloroperbenzoic acid

m-chlorobenzoic acid

→

safrole oxide

Ausbeute 39.3%

Lösungsmittel

chloroform

chloroform

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwhile maintaining the temperature at 0° - 5° C
2. 2
   Filtrationwere filtered
3. 3
   Waschenthe filtrate was washed twice with 5% sodium hydroxide solution
4. 4
   TrocknenAfter drying over anhydrous sodium sulfate
5. 5
   Sonstigethe solvent was evaporated
6. 6
   Sonstigeto obtain the residue
7. 7
   workup.DISTILLATIONThis was distilled under reduced pressure

Vorschrift

16.2 g of safrole was dissolved in 100 ml of chloroform and to the mixture was added dropwise 20.7 g of m-chloroperbenzoic acid dissolved in 500 ml of chloroform at 0°-5° C. The resulting mixture was allowed to stand with slow stirring for 55 hours, while maintaining the temperature at 0° - 5° C. After the completion of the reaction, m-chlorobenzoic acid crystals were filtered and the filtrate was washed twice with 5% sodium hydroxide solution, and then with water. After drying over anhydrous sodium sulfate, the solvent was evaporated to obtain the residue. This was distilled under reduced pressure to give 7.0 g (yield 39.3%) of safrole oxide as colourless oily substance having a boiling point of 108° - 110° C/3 mmHg.

Quelle