Reaktion #5090

Reaktionsgleichung

2,3-dihydro-2,4-dimethyl-3-phenyl-7-hydroxy-1H-inden-1-one

crotyl bromide

potassium hydroxide

→

2,3-dihydro-2,4-dimethyl-3-phenyl-7-crotyloxy-1H-inden-1-one

Lösungsmittel

acetone

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturrefluxed
2. 2
   Einengenthe reaction mixture was concentrated
3. 3
   Extraktionextracted with ethyl acetate
4. 4
   Waschenthe extract was washed with water and with an aqueous solution saturated with sodium chloride
5. 5
   Sonstigedried
6. 6
   EinengenThe extract was concentrated
7. 7
   Sonstigeby removing the solvent under a reduced pressure
8. 8
   Sonstigerecrystallized from methanol

Vorschrift

A solution of 19.0 g of 2,3-dihydro-2,4-dimethyl-3-phenyl-7-hydroxy-1H-inden-1-one, 13.98 of crotyl bromide and 5.47 g of potassium hydroxide in 200 ml of acetone was heated and refluxed under stirring condition. After the reaction was completed, the reaction mixture was concentrated and extracted with ethyl acetate, then the extract was washed with water and with an aqueous solution saturated with sodium chloride, then dried. The extract was concentrated by removing the solvent under a reduced pressure, then recrystallized from methanol to obtain 11.8 g of 2,3-dihydro-2,4-dimethyl-3-phenyl-7-crotyloxy-1H-inden-1-one as in the form of cis-trans mixture. Colorless stick-like crystals. Melting point: 138.5°-139.5° C.

Quelle