반응 #654322

ord-843ec1df30db4c12be592c5d9ec3e4b4

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONdropwise and during the course of addition, temperature
  2. 2
    기타was kept no higher than 25° C., while the mixture
  3. 3
    기타the phases were separated
  4. 4
    세척the organic phase was washed with water three times
  5. 5
    기타dried
  6. 6
    농축concentrated

실험 절차

In a 250 ml single neck flask was charged 12.4 g (100 mmoles,1.0 eq) of 4-fluorobenzaldehyde dissolved in 30 ml of acetone. To this was added 5 g of 10% aqueous sodium hydroxide solution (12.5 mmoles, 0.125 eq), dropwise and during the course of addition, temperature was kept no higher than 25° C., while the mixture was agitated continuously for 30 minutes. To the mixture was added 50 ml of water, followed by 100 ml of ethyl acetate, the phases were separated and the organic phase was washed with water three times and then dried, and concentrated to obtain 13.5 g of 4-(4-fluorophenyl)-3-buten-2-one as a faintly yellow oil in 82.3% yield.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06177462B1uspto-grants-2001_01