تفاعل #5090

ord-052823d5aace48c1ba767bdcf24f3608

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةrefluxed
  2. 2
    تركيزthe reaction mixture was concentrated
  3. 3
    استخلاصextracted with ethyl acetate
  4. 4
    غسيلthe extract was washed with water and with an aqueous solution saturated with sodium chloride
  5. 5
    أخرىdried
  6. 6
    تركيزThe extract was concentrated
  7. 7
    أخرىby removing the solvent under a reduced pressure
  8. 8
    أخرىrecrystallized from methanol

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05242919uspto-grants-1993_09