反応 #79761

ord-7fe1ab5cd2914eb199377ade391620fb

反応条件

温度
120°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The mixture was cooled to ambient temperature
  2. 2
    ろ過filtered
  3. 3
    workup.ADDITIONWater (500 ml) was added to the filtrate
  4. 4
    抽出the mixture was extracted with ethyl acetate
  5. 5
    その他to give a solid which
  6. 6
    その他was triturated with hot hexane (500 ml)
  7. 7
    その他The supernatant liquid was decanted from a residual gum
  8. 8
    温度cooled
  9. 9
    その他The solid which precipitated
  10. 10
    ろ過was collected by filtration

実験手順

A mixture of 4-iodophenol (25.0 g), 2-fluorobenzaldehyde (14.14 g), potassium carbonate (31.5 g) and dimethylformamide (500 ml) was heated at 120° C. under nitrogen with stirring for 15 hours. The mixture was cooled to ambient temperature and filtered. Water (500 ml) was added to the filtrate and the mixture was extracted with ethyl acetate to give a solid which was triturated with hot hexane (500 ml). The supernatant liquid was decanted from a residual gum and cooled. The solid which precipitated was collected by filtration to give 2-(4-iodophenoxy) benzaldehyde, m.p. 84.5-86° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06713474B2uspto-grants-2004_03