반응 #42738

ord-fa224b4cc0cd49ce92d0db54d17f8641

반응 조건

온도
140°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The reaction mixture is cooled to room temperature
  2. 2
    workup.ADDITIONpoured onto ice-water
  3. 3
    추출extracted with methylene chloride
  4. 4
    세척The organic layer is washed with saturated sodium hydrogen carbonate solution
  5. 5
    건조dried over anhydrous magnesium sulfate
  6. 6
    기타evaporated to dryness in vacuo

실험 절차

A mixture of 2-(4-chlorophenyl)-1-(3,4-difluoro-2-hydroxy-phenyl)-4-methyl-pentane-1,3-dione (3.65 g, 10.3 mmol) in acetic acid (36 ml) and concentrated HCl solution (2 ml) is stirred at 140° C. for 3 h. The reaction mixture is cooled to room temperature, poured onto ice-water and extracted with methylene chloride. The organic layer is washed with saturated sodium hydrogen carbonate solution, dried over anhydrous magnesium sulfate and evaporated to dryness in vacuo to afford the title compound as a brown solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07732435B2uspto-grants-2010_06