반응 #5090

반응 방정식

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

용매

acetone

반응 조건

후처리

1. 1
   온도refluxed
2. 2
   농축the reaction mixture was concentrated
3. 3
   추출extracted with ethyl acetate
4. 4
   세척the extract was washed with water and with an aqueous solution saturated with sodium chloride
5. 5
   기타dried
6. 6
   농축The extract was concentrated
7. 7
   기타by removing the solvent under a reduced pressure
8. 8
   기타recrystallized from methanol

실험 절차

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.

출처