反応 #742252

ord-ff72df1e00034eddb3180f5fcfb72700

反応方程式

CCOC(=O)C=Cc1ccccc1O
3-(2-hydroxy-phenyl)-acrylic acid ethyl ester
C=CCCCCCCCCO
dec-9-en-1-ol
C=CCCCCCCCCOC(=O)/C=C/c1ccccc1O
colourless crystals
収率 21.5%
C=CCCCCCCCCOC(=O)/C=C/c1ccccc1O
(E)-3-(2-Hydroxy-phenyl)-acrylic acid dec-9-enyl ester
収率 21.5%

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: USRE043006E1uspto-grants-2011_12