反应 #742252

ord-ff72df1e00034eddb3180f5fcfb72700

反应方程式

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

溶剂

反应条件

温度
150°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: USRE043006E1uspto-grants-2011_12