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

HRID 655070

반응식

HRID 655070 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
150 °C

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ff72df1e00034eddb3180f5fcfb72700
출처 데이터셋
uspto-grants-2011_12
특허 번호
USRE043006E1

연결된 노트

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