反応 #55326

ord-d793c88c8d7b496f95f1650ed93717a2

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONwas added dropwise
  2. 2
    workup.ADDITIONwas added to the stirred suspension
  3. 3
    workup.DISSOLUTIONto dissolve the gummy precipitate which
  4. 4
    その他formed and after an additional 15 minutes
  5. 5
    その他(after about 2 hours)
  6. 6
    抽出was extracted with additional ether
  7. 7
    洗浄the combined ether extracts were washed with water
  8. 8
    その他evaporated
  9. 9
    乾燥after drying with Na2SO4

実験手順

The keto-ester III (143.8 g) was stirred in dilute formaldehyde solution (62 ml 37% formaldehyde+water 220 ml) and to the suspension potassium carbonate solution (54.5 g, in water 280 ml) was added dropwise. At the end of the addition, ether was added to the stirred suspension to dissolve the gummy precipitate which formed and after an additional 15 minutes, gas evolution commenced. When this gas evolution ceased (after about 2 hours) the reaction mixture was extracted with additional ether and the combined ether extracts were washed with water and evaporated after drying with Na2SO4. The yield of the ethyl-2-(p-ethoxyphenyl)acrylate (II) (isolated as a yellow oil) was 97.8 g (79.8%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04220591uspto-grants-1980_09