9-Decen-1-ol → 2-Propenoic acid, 3-(2-hydroxyphenyl)-, 9-decen-1-yl ester, (2E)-

HRID 655070

反応式

HRID 655070 の反応式
[CH2:1]([O:3][C:4](=[O:14])[CH:5]=[CH:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[OH:13])[CH3:2].[CH2:15](O)[CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22]C=C>CCOCC>[CH2:1]([O:3][C:4](=[O:14])/[CH:5]=[CH:6]/[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[OH:13])[CH2:2][CH2:22][CH2:21][CH2:20][CH2:19][CH2:18][CH2:17][CH:16]=[CH2:15]

参加物

4

反応物 2

HCID 256129-Decen-1-olHCID 576496Ethyl 3-(2-hydroxyphenyl)prop-2-enoate

生成物 1

HCID 177820092-Propenoic acid, 3-(2-hydroxyphenyl)-, 9-decen-1-yl ester, (2E)-収率 21.5%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
150 °C

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.

後処理

  1. customremoving the ethanol
  2. customformed
  3. temperaturethe reaction mixture was cooled
  4. washwashed with brine
  5. customThe organic phase was dried
  6. customevaporated to dryness
  7. distillationThe resulting oil was Kugelrohr-distilled
  8. customcrystallized
  9. customrecrystallized

出典と根拠

ORDレコード
ord-ff72df1e00034eddb3180f5fcfb72700
出典データセット
uspto-grants-2011_12
特許番号
USRE043006E1

関連ノート

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