반응 #742252

ord-ff72df1e00034eddb3180f5fcfb72700

반응 방정식

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
수율 21.5%
C=CCCCCCCCCOC(=O)/C=C/c1ccccc1O
(E)-3-(2-Hydroxy-phenyl)-acrylic acid dec-9-enyl ester
수율 21.5%

용매

반응 조건

온도
150°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타removing the ethanol
  2. 2
    기타formed
  3. 3
    온도the reaction mixture was cooled
  4. 4
    세척washed with brine
  5. 5
    기타The organic phase was dried
  6. 6
    기타evaporated to dryness
  7. 7
    workup.DISTILLATIONThe resulting oil was Kugelrohr-distilled
  8. 8
    기타crystallized
  9. 9
    기타recrystallized

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: USRE043006E1uspto-grants-2011_12