反応 #1957759

ord-af660bd7cf184a139868a73e7f4c1c21

溶媒

反応条件

温度
150°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他removing the ethanol
  2. 2
    その他formed
  3. 3
    温度the reaction mixture was cooled
  4. 4
    洗浄washed with brine
  5. 5
    その他The organic phase was dried
  6. 6
    その他evaporated to dryness
  7. 7
    workup.DISTILLATIONThe resulting oil was Kugelrohr-distilled
  8. 8
    その他crystallized
  9. 9
    その他recrystallized

実験手順

A mixture of 5.0 g 3-(2-hydroxy-phenyl)-acrylic acid ethyl ester, 6.1 g dec-9-en-1-ol and 1.0 g tetraisopropyl-ortho-titanate was heated to 150° C. removing the ethanol formed. After stirring for 2.5 hours at this temperature, the reaction mixture was cooled, diluted with ether and washed with brine. The organic phase was dried and evaporated to dryness. The resulting oil was Kugelrohr-distilled, crystallized and recrystallized to yield 1.69 g of colourless crystals.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06096918uspto-grants-2000_08