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2-Propenoic acid, 3-[4-(trifluoromethyl)phenyl]-, ethyl ester → (E)-3-(4-(trifluoromethyl)phenyl)prop-2-en-1-ol

HRID 661064
ノート
印刷プレビュー

反応式

HRID 661064 の反応式
[F:1][C:2]([F:17])([F:16])[C:3]1[CH:8]=[CH:7][C:6](/[CH:9]=[CH:10]/[C:11](OCC)=[O:12])=[CH:5][CH:4]=1.[H-].C([Al+]CC(C)C)C(C)C>CCOCC.CCCCCC>[F:1][C:2]([F:16])([F:17])[C:3]1[CH:4]=[CH:5][C:6](/[CH:9]=[CH:10]/[CH2:11][OH:12])=[CH:7][CH:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 115070152-Propenoic acid, 3-[4-(trifluoromethyl)phenyl]-, ethyl esterHCID 21225700Diisobutylaluminumhydride

生成物 1

HCID 10512285(E)-3-(4-(trifluoromethyl)phenyl)prop-2-en-1-ol収率 74.2%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8058Hexane溶媒

実験手順

(E)-Ethyl 3-(4-(trifluoromethyl)phenyl)acrylate (25.00 g, 102 mmol) in 100 mL ether was cooled in an ice-water bath. To this solution, di-iso-butylaluminum hydride (205 mL, 205 mmol) in hexane was added. After addition, the ice-water bath was removed. After 2 hours of stirring at room temperature, the reaction mixture was diluted with 200 mL diethyl ether, cooled to 0° C. and quenched with careful addition of 200 mL brine and 200 mL of 5.0 M HCl. The aqueous solution was extracted with diethyl ether twice (200 mL each time). The combined organic phases were washed with brine and dried over sodium sulfate. The product was chromatographed eluting with 20% EtOAc in hexane. After removing the solvent, a white solid was obtained as the desired product (15.3 g, yield=74%). 1H NMR (400 MHz, CD3OD) δ ppm 4.28 (dd, J=5.28, 1.57 Hz, 2H) 6.55 (dt, J=15.94, 5.23 Hz, 1H) 6.67-6.75 (m, 1H) 7.58-7.67 (m, 4H).

後処理

  1. additionAfter addition
  2. customthe ice-water bath was removed
  3. additionthe reaction mixture was diluted with 200 mL diethyl ether
  4. temperaturecooled to 0° C.
  5. customquenched with careful addition of 200 mL brine and 200 mL of 5.0 M HCl
  6. extractionThe aqueous solution was extracted with diethyl ether twice (200 mL each time)
  7. washThe combined organic phases were washed with brine
  8. dry with materialdried over sodium sulfate
  9. customThe product was chromatographed
  10. washeluting with 20% EtOAc in hexane
  11. customAfter removing the solvent

出典と根拠

ORDレコード
ord-a73c01f3601746a2a7fc57462ef66946
出典データセット
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08084479B2

反応ノート

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