反应 #5090

ord-052823d5aace48c1ba767bdcf24f3608

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度refluxed
  2. 2
    浓缩the reaction mixture was concentrated
  3. 3
    萃取extracted with ethyl acetate
  4. 4
    洗涤the extract was washed with water and with an aqueous solution saturated with sodium chloride
  5. 5
    其他dried
  6. 6
    浓缩The extract was concentrated
  7. 7
    其他by removing the solvent under a reduced pressure
  8. 8
    其他recrystallized from methanol

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05242919uspto-grants-1993_09